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Message from Secretary General, QCI . . . . . . . . . . . . . . . . . 6

ISO Workshop details . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-9

List of Governing Council . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Editor's Desk . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

Importance of Residue Study . . . . . . . . . . . . . . . . . . . . 12-14

Guidelines for Measurement of Mass in

Medical Calibration Laboratories . . . . . . . . . . . . . . . . . 15-17

ILAC Meeting, Frankfurt, Germany . . . . . . . . . . . . . . . . 18-19

Technical News . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20, 25-28

Quality Control systems in medical laboratories

Let us get a grip on them. . . . . . . . . . . . . . . . . . . . . . . . 29-30

Recent Trends in analysis of Vitamins . . . . . . . . . . . . . . 31-32

Trade News . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33-35

Basics of Internal Audit . . . . . . . . . . . . . . . . . . . . . . . . . 36-37

Member's Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38-40

AOIL Subscription form. . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

Anulab. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

Belz Instruments Pvt. Ltd. . . . . . . . . . . . . . . . . 3

ELCA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

SCC IT Solutions . . . . . . . . . . . . . . . . . . . . . . . 21

SGM Lab Solutions Pvt. Ltd.. . . . . . . . . . . . 22-23

Calitech . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Perfect Researchers Pvt. Ltd. . . . . . . . . . . . . . 42

DVG Laboratories . . . . . . . . . . . . . . . . . . . . . . 43

Farelabs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

April - June 2016, (Volume-1, Issue-2)AOIL BULLETIN 6

Message from Secretary General, QCI

(Dr. R. P. Singh)

As we all are aware, the importance of the laboratory comes from the fact that testing and calibration are vital components of any effective quality system. Quality cannot be achieved without measurement and quantification which is provided through a laboratory.

The awareness about the importance of laboratories and production of accurate and reliable results have gained importance over the past few years especially in recent times in context of global trade and commerce. For an economy to surge forward, there is a need to establish world class laboratories which will cater to the sophisticated needs of measurement in key emerging sectors like aerospace, defence, pharmaceuticals, biotechnology etc.

More importantly, it is important that the human resource employed in such laboratory understand the international standards so that they internalize their functions fully aligned to the laid down requirements. It becomes a matter of pride and encouragement, when these professionals are given an opportunity to be part of the process of either the development or revision of a standard.

I congratulate Association of Indian Laboratories (AOIL) for providing such an opportunity by organizing a country wide consultation along with NABL for gathering inputs of the stakeholders as the revision of ISO/IEC 17025:2005 is on the anvil. Probably, this is for the first time that the key stakeholders i.e. the laboratories who have to implement the standard are coming together in a big way to participate in the revision of this standard.

This consultation is apt and timely as it will give an opportunity to submit the inputs of the Indian Stakeholders in strengthening the standard for making it more pertinent to the needs of the Indian industry and make it more focused to realize the quality objectives. It is also a matter of privilege that in this endeavor of putting forth the Indian perspective, no less than the Chair of ILAC Mr. Peter Unger and WG 44 member Mr. Jeff Gust have been roped for this pioneering effort. I welcome them and thank them for graciously accepting and supporting India to this noble cause.

I also take this opportunity to extend all support of the Quality Council of India to strengthen the quality ecosystem by professing the use of third party certification, testing and calibration in all facets of quality intervention.

We all understand that India is strongly surging ahead with a multitude of activities including the initiative of Make in India which emphasizes on ZERO DEFECT and ZERO EFFECT has given further impetus to strengthening and upgradation of laboratories across various sectors.With this, I once again thank AOIL for organizing this function and urge all the experts from various laboratories from all over the country and beyond to participate with full enthusiasm so that it becomes a SUCCESS.


"WORKSHOP ON ISO/IEC 17025 REVISION"

Association of Indian laboratories (AOIL), in collaboration with National Accreditation Board for testing and calibration (NABL)is organising workhops to focus on changes proposed in the International Standard ISO/ IEC 17025and also to seek feedback from laboratories for its consideration by ILAC &CASCO working Group-44. In the process of the revision of the standard it is subjected to debate world over and these workshops are being organised to give exposure to the Indian Laboratories with the process of development of International Standards which is of prime concern of AOIL.

Eminent speakers have been invited to attend the workshop :-

Mr. Peter Unger Chairman ILACMr. Jeff Gust Member of CASCO WORKING group-44Mr. D. S. TEWARI Chairman – AOIl

Three workshops have been planned at New Delhi, Mumbai and Bangalore on 14th , 15th and 16th April 2016 respectively. Senior Technical and Quality Managers are invited from the Accredited laboratories for participation , so that a fruitful discussions can be held during the session. The activity would be the first of its kind where the experts from laboratories would be interacting with the International experts Mr. PETER UNGER and Mr. JEFF GUST.

Participation ,is of more significance , keeping in mind that all laboratories would have to undergo similar training to understand the changes in the standard. The participant will get the training from International Experts and receive a Certificate of participation after completing the workshop.

AOIL believe that this is a rare opportunity where laboratories give their inputs in the International Standards and put forward the difficulties being experienced in acquiring and maintaining the Accreditation.

WORKSHOP SCHEDULEDATE: 14th April 2016

VENUE: HOTEL HOLIDAY INN, AERO CITY , TERMINAL-3 DELHI AIRPORT, NEW DELHI

Time Activity Involving

0830 hrs. to 0930 hrs Registration ALL

0930 hrs. to 1030 hrs. Inaugural Session ALL

1030 hrs. to 11.00 hrs. TEA ALL

11.00 hrs. to 11.05 hrs. History of laboratory criteria Devi Saran Tewari

11.05 hrs. to 11.15 hrs. Introduction of CD-2 17025 Peter Unger

11.15 hrs. to 13.00 hrs. Presentation of CD 2 17025 JEFF GUST

1300 hrs. to 1400 hrs. LUNCH All are Invited

1400 hrs. to 1600 hrs. Open house Peter Unger, Jeff Gust

Anil Relia, D.S. Tewari

1600 hrs. to 1630 hrs. Tea ALL

1630 hrs. to 1730hrs. Concluding Session and vote of thanks. ALL

Note. : 1. Concluding session to focus on summarization of the views of the participants onISO/IEC 17025, CD-2, to communicate to ILAC and WG44, by AOIL and NABL.

2. Inaugural session details would be given on the day of workshop.

ASSOCIATION OF INDIAN LABORATORIES

LIST OF GOVERNING COUNCIL MEMBERS AND OFFICE BEARERSFOR THE PERIOD 2015-2017.

1. Sh. D. S. TEWARI CHAIRMAN 9968151381

2. Sh. A. K. NEHRA PRESIDENT 9810197068 [email protected]

3. Sh. RAJESH DESWAL SECY. GENERAL 9811787807 [email protected]

4. Sh. VIVEK BAGGA VICE PRESIDENT 9811672278 [email protected](CALIBRATION)

5. Dr. R. B. SINGH VICE PRESIDENT 09837052O93 [email protected](TESTING)

6. Dr. S.Y. PANDEY VICE PRESIDENT 09909900919 [email protected](GLP)

7. Dr. ALOK AHUJA VICE PRESIDENT 09837009700 [email protected](MEDICAL)

8. Sh. K. DHINGRA JT. SECRETARY 9873001515 [email protected]

9. Sh. KAPIL VASHIST TREASURER 9810088217 [email protected]

10 Sh. D. MATHUR CHAIRMAN( N.R ) 9312664533 [email protected]

11 Sh. N. KALYAN CHAIRMAN(W.R.) 09821056975 [email protected]

12. Sh. SHASHI KUMAR CHAIRMAN(S.R) 9972697755 [email protected]

13. Sh. C.S. JOSHI EDITOR 9313066685 [email protected]

14. Dr. NEERAJ JAIN MEMBER 9810492621 [email protected]

15. Sh. LALIT PANERI MEMBER 9829043949 [email protected]

16. Sh. GAURAV TEWARI MEMBER 9811893191 [email protected]

17. Sh. ARUN R. FREDICK MEMBER 9841085876 [email protected]

18. Sh. R.C. ARORA EXEC.SECRETARY 9599056365 [email protected]

[email protected]


Compliance to the prescribed standards is a basic requirement of operators of

quality assurance and quality control business. Though many quality operators see

adherence to the rule book as a burden but observance and adherence to the quality

guidelines ensure smooth and profitable operations. In the process of attaining

various accreditations, testing organizations not only acquire cutting edge

competence and expertise but also develop pool of talented and competent manpower,

which help the organization in long run.

Organizations capability for adherence to the compliance, demonstrate its

control over unit operations, systems, processes, safety, quality and reliability of

results. It also spread message among clients, customers, regulators and stake holders

that the organization is honest, capable and responsible business entity.

The awareness about safety and standard in lab operation is increasing day

by day. The outcome is positive and India is witnessing more reliable and responsible

quality assurance and quality control environment. This will help us in our integration

with international counterparts and will open new horizon of business opportunities.

This will also help us in emerging as reliable international quality testing destination.

AOIL is eager to spread this message far and wide among all stake holders,

international quality and business entities. In this connection AOIL with NABL and

QCI has invited international experts Mr. Peter Unger, chair ILAC and Mr. Jeff Gust,

member WG 44. All the laboratories in India and in neighboring countries will have

good opportunity to participate and contribute their input in development of

international standard. This will help our laboratories to achieve and realize their full

potential and will help them to make their presence felt on international quality

platform.

Yours truly

C S Joshi

Editor


d. Confirmation

RESIDUE TRIAL• Required as part of the authorization procedure for

plant protection products; this is normally achieved by undertaking supervised trials

• Field of use : Use of the plant protection products (for instance field use, protection crops etc.)

• Mode of application : On specified agricultural commodities, against identified harmful organisms, purpose of use, timing, rate and number of application

• Area of application : Agriculture, horiculture, viticulture, home garden, forestry and cultivation of hops

• Size of area will vary crop to crop, should be large enough to avoid contamination during sampling and harvesting

• Control plot should be sited immediate vicinity of the treated area, but avoiding spray drift/cross contamination

• Harvest level : Residue level at time of harvest

• Residue decline studies : Five sampling stages, two of which are frequently set to coincide with the time of application and the harvest respectively

• Pre-Harvest interval (PHI) must be declared

RESIDUE TRIAL – APPLICATION• Trial based on proposed/approved rate of

application

• Water volume may differ, should be recorded

• When preparing spray solution precise attention should be paid to the specified dose level – adventitious dipping at turning point, under dosing because of drifting, should be avoided

• Residue trial should reflect the proposed critical GAP (Good Agricultural practice) (Number of application, interval and timing of application

• Sowing time, may indicate whether a given variety may be harvested early or late.

• Differential growth rates involved may affect residue behaviour to a different extent

• For crops with extended harvest periods records on harvest should include beginning and end of harvest

• Information on weather immediately after application and on the day of application are most important, Special attention should be accorded to

IMPORTANCE OF RESIDUE STUDYS.T.Maheswari, Ph.D., MRQA, ICSQA

QA ManagerInternational Institute of Biotechnology and Toxicology (IIBAT)Padappai-601 301, Kancheepuram District, Tamil Nadu, India.

Evaluation of pesticide residues in environmental, agricultural and food commodities are the dosimeters of the likely exposure by the individual or the commodity. The JMPR ( Joint meeting on Pesticide Residues ) is a systematic evaluation process that involves world wide multisite screenings recommends the actual MRL values for different crops relevant to the pesticides. The presence and or absence of a pesticide residue attracts greater consumer interest.Consumer are aware of the consequence of the pesticides and their residues at trace levels. It is the responsibility of the residue chemist to establish the truth in the analysis.

The major problem associated with the pesticide residue analysis is the matrix interference.

The challenging task is answering the question : The absence of residues is due to non availability of residues or due to lack of sensitivity of the technique /method used.

The challenging task is the answering the question : The absence of residues is due to non availability of residues or due to lack of sensitivity of the technique/method used. Similarly the presence of residues: Is it due to actual presence of the chemical or due to relevant spike. That is the reason US EPA made the confirmation of residue analysis by GC-MS/LC-MS/MS a mandatory. In this process of evaluation Good Laboratory Practices (GLP) attained critical importance. The purpose of practicing GLP principles in a study is for getting the global acceptance of the data generated by an individual country/laboratory.

Unless otherwise specified by any individual countries these principles are intended for non clinical health and environmental studies.

Purpose of residue studies/Crop residue studies

It is a part of field study that involves more analytical. The main purpose of the residue study is : to fix MRL and ADI ( Global ) and to fix Waiting period and PHI (local). The guidelines to follow are SANCO, GAP and GLP.

Basic Parameter in Pesticide Residues Analysis

Pesticide Residues Analysisa. Sampling

b. Analytical tools

c. Quantification



• Range appropriate to the lowest and highest nominal concentration of the analyte + at least 20%

• Either duplicate of 3 or 4 concentrations or single determination of 5 or more concentrations

• Matrix matched standards where appropriate

• Statistical parameters – correlation coefficient

LIMIT OF DETECTION – LOD• The lowest concentration detectable by the

instrument with the S/N ratio 3:1 – means 3 times greater than noise level

• LOD has no fixed value

• Restricted to the response of the detection system and applicable to the complete analytical method

ACCURACY/RECOVERY• Determination of accuracy may be based on the

recovery of known amounts of analyte from a representative sample matrix

• Two concentrations (LOQ level & 10XLOQ level), 5 replications and 2 controls of each matrix

• Acceptable range of recovery % = 70-110, ideally 80-100%

PRECISION-REPEATABILITY (r)• The closeness of agreement between independent

test results obtained under prescribed condition

• Minimum 5 or 7 at each fortification level

• Statistical parameters – Relative standard deviation (RSDR) ; Acceptance based on Horwitz equation, depends on analyte concentration

• Horwitz equation RSD < 2(1-0.5 logC) x 0.67 (C-Concentration of analyte)

SUGGESTED MAXIMUM RSD AS A FUNCTION OF ANLAYTE CONCENTRATION

Analyte % Analyte Ratio - C Unit RSD%

100 1 100% 1.34

10 10-1 10% 1.89

1 10-2 1% 2.68

0.1 10-3 0.1% 3.79

0.01 10-4 100 ppm 5.36

0.001 10-5 10 ppm 7.58

0.0001 10-6 1 ppm 10.72

0.00001 10-7 100 ppb 15.16

0.000001 10-8 10 ppb 21.44

0.0000001 10-9 1 ppb 30.32

LIMIT OF DETERMINATION/LIMIT OF QUANTIFICATION – LOQ• Defined as the lowest concentration tested, at which

an acceptable mean recovery with an acceptable

the period intervening between application and harvest

Residue studies – Critical phases• Soil History

• Plot design

• Calibration of spray equipment

• Spray personnel calibration

• Wind influence

• Spray fluid stability

• Tank cleaning studies

PESTICIDE RESIDUES - REQUIREMENTS• METHOD VALIDATION

• RESIDUE TRIAL

• SAMPLING

• CONTAMINATION AND INTERFERENCE

References• SANCO/825/00 rev.6

• Directive 91/414/EEC

Development of Validated Analytical MethodValidation has been defined as the process of determining the suitability of methodology for providing useful analytical data.

Stage 1 Estimation of acceptable performance parameters within a laboratory

Stage 2 Demonstration of successful performance in limited interlaboratory studies.

Stage 3 Demonstration of successful performance in recognized collaborative study

Stages in method development

• ELEMENTS OF METHOD VALIDATION

• CALIBRATION

• LIMIT OF DETECTION – LOD

• ACCURACY/RECOVERY

• PRECISION/REPEATABILITY

• L IMIT OF DETERMINATION/L IMIT OF QUANTIFICATION – LOQ

• SPECIFICITY

• CONFIRMATION

CALIBRATION• The ability of detection system, within defined

range, to produce an acceptable linear correlation between the test results and the concentration of analyte in the sample


RSD, is obtained

• LOQ = 3 x LOD

• S/N ratio : minimum 10:1 with acceptable precision and recovery of analyte

• LOQ < MRL, NOEL or LC50, NOEC or EC50

• LOQ in water - < 0.1 µg/L (EU DRINKING WATER SPECIFICATIONS)

• Surface water – not exceed a concentration which has an impact on non-target organisms

• LOQ for residue in air < C

• C= AOELinhalative * 0.1* 60/20 (mg/m3 air)

• Where, 0.1 - Safety factor

• 60 – body weight in Kg

• 20 – Air intake per day in m3

SPECIFICITY• The ability of a method to distinguish between the

analyte being measured and other substances, based upon sufficient characteristics of the analyte as to make the results completely specific to the analyte, irrespective of the characteristics of other materials

• CONFIRMATION OF RESIDUE(S)

• Required to demonstrate specificity,

• Not required where primary method is shown to be specific to the analyte of interest

• GC-MS/LC-MS : at least 3 fragment ions with an m/z ration of >100

• HPLC-DAD, if the UV spectrum is characteristics

• Alternative detection

• Derivatisation, if it was not first choice of the method

• Different stationary phase/mobile phase of different selectivity

SAMPLING• Systematic sampling methods – “X” and “S”

• pattern – starting from the edge of the plot

• A distinction is to be made between test

• and control samples

• Sampling – Control followed by test samples

• Contamination - hand, cloth, during transportation must be avoided

• Should be clearly labelled and packed – Storage at -18°C

• Stability of compound should be checked by spiking standard in control during storage at -18°C

• Sampling dates are dependent on previous knowledge of the stability of the residues

EXTRACTION & CONCENTRATION• Test portions should be disintegrated thoroughly

during extraction to maximise extraction efficiency (where ever applicable)

• When extracts are evaporated to dryness, use a small volume of high boiling point solvent as a “KEEPER” & Keep temperature as low

• A stream of nitrogen or vacuum centrifugal evaporation is generally preferable for small scale evaporation

• Calibrated vessels of not < 1ml should be used

• Analyte stability in extracts should be investigated during method validation

CONTAMINATION & INTERFERENCE• Store samples separately from other sources of

potential contamination

• All equipments must be cleaned scrupulously, especially for re-use

• Where an internal standard is used, unintended contamination of extracts or analyte solutions with the internal standard, or vice versa, must be avoided

• If the interference takes the form of a response overlapping that of the analyte, a different clean-up or determination system may be required

MAXIMUM RESIDUE LEVEL (MRL)• Maximum residue levels are set on the basis of

supervised trials in which GAP is observed and must not pose an unacceptable risk to human health

• Experience has shown that statistical methods have proved to be useful tools in the derivation of MRL but these should not replace scientific judgement bases on all available data

• Formula for calculating the proposed MRL

R(ber): 2*R(0.75) = 2*[(1-G)*R(J)+G*R(J+1)]

Where,

G - fraction of (n+1) *P

R(J) – Residue valued at point J

J – Whole integer proportion of (n+1)*P

ACCEPTABLE DAILY INTAKE (ADI)• ADI of chemical is the daily intake, which during an

entire lifetime, appears to have no appreciable risk to the health of the consumer on the basis of all the known facts at the time of the evaluation of the chemical

• ADI = NOAEL animal studies (mg/kg body weight/day)/100(safety factor)

NOAEL = No-observed adverse effect level

Measurements (DCM) used to determine the mass in medical/Pharmaceutical measurement laboratories, specified method for determination of the relative expanded uncertainty of the estimated mass of any product weighed, have been covered in this paper.

Weighing in Medical/Pharmaceutical Company

For a small Medical/Pharmaceutical company, the activities of all the three sectors i.e. the Research and Development Sector, Primary Operation Sector and Secondary Manufacturing Operations Sector, may be co-located. But for a larger company, the three operations may be performed on separate sites and for multinational companies may be spread over several countries. During all of these operations a large number of weighings are to be performed using standard weights of highest accuracy class and a wide range of balances and scales.

The Advisory Council for Metrology in Medicine the Physikalisch-Technische Bundesanstalt (PTB) published a “Guide for the determination of the mass within the scope of reference measurement procedures in medical reference measurement laboratories”[4]. This Guide establishes metrological requirements for the calibration of measuring devices used to determine the mass within the scope of calibration procedures in medical reference measurement laboratories. The requirements mentioned in following sections are based on this guide.

Required Standards Weights

The weights required for determination of mass in various operations in Medical /Pharmaceutical Laboratories

must be standard weights to ensure traceability to the national standard which realizes the unit of mass in compliance with the International System of Units (SI)[3]. These weights must be accompanied by a calibration certificate issued by an accredited calibration laboratory or a national metrology institute (e.g. NPLI), or by a verification certificate stating the conventional masses [7] and associated uncertainties of measurement (U). All certificates must be kept for the whole period of use (service life) of these weights.

Guidelines for Measurement of Mass inMedical Calibration Laboratories

Tripurari LalEx. Scientist G & Head, Mass Standards

National Physical Laboratory New Delhi (India)E-mail: [email protected]

Introduction

The International Bureau of Weights and Measures defines metrology as the science of measurement, embracing both experimental and theoretical determinations at any level of uncertainty in any field of science and technology [1]. Measurements of physiological, biochemical, physical, and other patient-related variables are not only ubiquitous in intensive care medicine and beyond, but the results from such measurements also provide essential information for critical decision-making in clinical practice, as well as for research and technology development. Erroneous measurements can jeopardize patient safety and can expose the most critically ill patients to severe hazards. If physiological variables cannot be measured properly, then therapy-targeting changes in those variables, also, cannot be adjusted properly.

Physiological variables are associated and measured in terms of physical measurable quantities. A quantity is a property of a phenomenon, body, or substance, to which is attributed a magnitude that can be expressed as a number and a reference [2]. A reference can be a measurement unit, a measurement procedure, a reference material, or a combination of such. There are seven base quantities on which international quantities are based. These seven base quantities are listed in Ref. [3] with five other derived quantities (Force, Pressure, Work or Energy, Power & Frequency) often used in medicine.

The Mass in Medical Measurement Laboratories

The quantity Mass is one of the most importance base quantities of the international system of measurements. The measurement of mass, either directly or indirectly has always been affecting every activities of our everyday life. In addition to the direct impact on trade and commerce, mass measurements impact the scientific community as well as a broad range of manufacturing industries, including chemical, bio-medical and pathological test and calibration Laboratories. In various operations in such industries and laboratories a large number of weighings are performed using standard weights of highest accuracy class [5] and a wide range of weighing balances & scales. Based on various national/international guides, the metrological requirements for various Devices for Calibration &


The relative standard uncertainty urel, assigned to the conventional mass (m) of the standard weights should be equal to or smaller than one-sixth of the relative expanded uncertainty U/m, i.e. = 0.015 %. This requirement [8] is met for the accuracy classes of the weights [5] shown in Table 1.

The conventional mass stated in the certificate is usually taken into account. The relative standard uncertainty urel is calculated from the uncertainty of measurement US given in the calibration certificate of the standard weight, using given coverage factor k and the nominal value m0, as urel = Us/(k.mo)

The nominal value m0 may be used instead of the certified mass ms of the standard weight for the calculation of the uncertainty of measurement, as the difference between ms and m0 is negligible here. In some cases, if more than one weight is used as a standard, the uncertainties assigned to the conventional masses of the individual weights must be linearly added because correlations exist between them to calculate:

The standard weights should be re-calibrated within a period not exceeding two years.. The recalibration period may be extended to maximum up to four years if there is an agreement with its previous mass values. If the change in its mass values exceed the uncertainty of measurement Us, the period must, be reduced to one year or other standards of better stability should be used or the conditions of use must be improved.

Prior to each use, the weights must be checked for any visible defects and contaminations. They may be used only if no significant changes in their mass values are noticed. The weights must be handled carefully, using suitable tweezers with plastic surfaces. Before each use, dust possibly adhering to them should be removed with a soft brush.

Required weighing instrument

The relative standard uncertainty urel,w of the mass value indicated by the weighing instrument contributes the greatest uncertainty to the determination of the mass within the scope of reference measurement procedures in medical calibration laboratories. As per USP 41[8], it must be smaller than half the relative expanded uncertainty of 0.10 %.. The relative standard uncertainty urel,w is given by the formula,

Recommended electronic weighing instruments which usually meet the above requirements are given in the Table 2 below:Table 2

Determination of the Repeatability of the Weighing Instrument

The measure of the repeatability of the weighing instrument is the standard deviation sw of the repeated indications of its scale at the desired load. The method for the determination of this standard deviation is being described here. The measurement sequence followed, to determine the standard deviation sw, must be in accordance with the measurement sequence followed in practical application. At least ten repeated measurement are taken in the following steps:

• Place the container on the balance pan, tare the balance and read the balance indication I1.

• Place the container and standard weights of total mass equal to the mass of the quantity to be weighed and then read the balance indication I2.

Repeat above steps several times (normally ten times) to determine ten such differences di (i = 1 to n). Each time the tare container is placed on the weighing instrument, the instrument’s indication is set to zero.

The standard deviation sw is calculated using following formula:

The load is to be applied to the balance pan in the same way as in actual weighing. Special care is taken to minimize the deviation of the load from the center of the pan during loading to keep the uncertainty contribution due to eccentric loading negligibly small. The influence of the remaining positional error, which cannot be avoided, included in the standard deviation determined above.

Linearity of the weighing instrument’s indication

The sequence for the determination of the correctness (linearity) of the indications of the weighing instrument should also be in compliance with the weighings carried out to determine the mass of the weighed quantities. In the range of the maximum weighing difference (e.g. 250 mg), the deviation of the weighing instrument’s indication from the conventional mass of the weights should be


smaller than the standard deviation sw. If this deviation is more than sw the linearity correction has to be applied in the observed mass or this deviation has to be taken into account by an additional uncertainty component, treating as rectangular distribution.

The weighing instrument must be calibrated and documented at least once in a year.

Environmental conditions

The environmental conditions during the measurement should meet requirements of the manufacturer of the weighing instrument or it should be maintained as given in the Table 3.

Determination of Mass

Before using the weighing instrument, adjust it in accordance with the instructions of the Manufacturer. Gross deviations due to eccentric loading must be avoided during weighing. The determination of mass of the object to be weighed is carried out in the following steps:

• One hour before the weighing process is started tare container and weights are placed on the pan of the weighing instrument to reach temperature stabilization.

• Set the zero of the weighing instrument by tarring with tare container

• Calibrate the weighing instrument in the measuring range used, with calibrated weights. The deviations of the masses of the standard weights from their respective nominal value should be smaller than the standard deviation sw of the weighing instrument.

• Again set the zero of the weighing instrument by tarring with tare container.

• Weigh the tare container with the substance to be weighed-in and determine the weighing result ( scale reading) mw .

Calculate the mass m.

The mass m is calculated according to equation (4) below, where mw is the indication of the weighing instrument for the weighed-in quantity. The conventional reference value of the air density is ?0 = 1,2 kg/m3 and the density of the standard weight used is ?s = 8000 kg/m3; the density ? of the product to be weighed must be known or assumed:

Calculation of the uncertainty

The relative expanded uncertainty U/m is determined from the relative standard uncertainties urel,w from the calibration of the weighing instrument used, the density of the product to be weighed and the coverage factor k = 2 according to the “Guide to the Expression of Uncertainty in Measurement” (JCGM 100:2008).

The relative standard uncertainty urel? of the density of the product to be weighed is calculated from the uncertainty u? of the density (?) of the product to be weighed. The uncertainty u? is calculated from the limiting values of the density, assuming rectangular distribution of density. If limiting value of the density of the product are ?max and ?min then the average value of the density of the product is given by ? = (?max+ ?min)/2 and the uncertainty, u? of this density is calculated as : u? = (?max - ?min)/ (2v3), assuming rectangular distribution.

The relative standard uncertainty of the density of the product to be weighed is urel? = u?/?. The relative standard uncertainty (urel) of the mass of the product weighed is given by:

The relative expanded uncertainty U/m of the mass of the object weighed is:

References

[1]. BIPM Website :http://www.bipm.org/en/worldwide-metrology/

[2]. JCGM 200:2012 International vocabulary of metrology (VIM) 3rd edition

[3]. The International System of Units Supplement 2014: Updates to the 8th edition (2006) of the SI Brochure.

[4]. PTB-Mitteilungen 109 (1999) No. 5, pp. 379-383.

[5]. OIML R 111: Weights of accuracy classes E1, E2, F1, F2, M1, M2, M3.

[6]. JCGM 100:2008, Guide to the Expression of Uncertainty in Measurement,

[7]. OIML D 28 : Conventional value of the result of weighing in air.

[8]. USP General Chapters <41< and <1251>: Feb. 2013.



The following GC members attended various committees & WG meetings:

1. Mr. D. S. Tewari, Chairman- ILAC-AIC 2. Mr. A. K. Nehra, President- ILAC-LC

3. Mr. R. B. Singh, VP-Testing- ILAC-LC 4. Mr. Lalit Paneri, GC Member-ILAC-ARC

The delegates attended meetings & actively participated in the delibrations, discussion & case studies in the committee

meetings. AOIL presentation in LC was appreciated by LC Chair & members from EUROLAB, A2LA, AOAC, ISTA,

NCLS, MLSCN, SLAB & IAS as effective- relevent to LC proceedings, and as an acknowledgement to AOIL & its team

on LC, Mr. A. K. Nehra & Mr. R. B.Singh both have been nominated to a joint task group- JTF with IAF on cooperation

between ABs by the LC Chair on 2nd Apr’16.

AOIL team has two lunch meetings, one with ILAC Chair Mr. Peter Aunger on 1st Apr’16 & other with Mr. Jeff Gust- LC

member & member WG44. Programme for the three IEC/ISO 17025 CD2 workshops proposed on 14, 15 & 16th Apr’16

at Delhi, Mumbai & Bangalore were discussed and finalised.

President AOIL invited LC members, for the forthcoming Delhi Annual Meetings of IAF-ILAC and offered the hosptatlity

of AOIL as associated host organisation. A dinner meeting was organised with three QCI delegates & officers present in

Frankfurt & QCI has extended active association to AOIL for the Delhi IAF-ILAC Conference in Oct’16 at Hotel Lalit,

New Delhi.

The following photographs are few selected glimpses of the AOIL participation In the IAF-ILAC Mid-Term Meetings-

Frankfurt, Germany.

AOIL delegation has participated inIAF-ILAC Mid-Term Meetings, which were

held in Hotel Le-Meredian, Frankfurt, Germanyfrom 30th Mar’16 to 2nd Apr’16,

as stakeholder ILAC member from India.

FDA Offers Guidance for Blood

Establishments during Ebola Outbreaks

The US Food and Drug Administration (FDA) has

re leased new recommendat ions for b lood

establishments to implement additional screening

measures during Ebola virus outbreaks.

Background: Since the outbreak began in 2014, the

World Health Organization (WHO) estimates that there

have been more than 28,000 cases of Ebola, resulting in

11,314 deaths. The outbreak has proven particularly

difficult for health authorities to quell in Guinea, Sierra

Leone and Liberia. In November, WHO declared that

Ebola transmission had ended in Sierra Leone, and

Guinea discharged its last known Ebola patient, a baby

girl, from the hospital. However, in the same month three

new cases of Ebola were reported in Liberia, where

WHO has twice declared transmission had stopped, in

May and September 2015.

While WHO has spearheaded the international response

to the outbreak, several US agencies including FDA, the

National Institutes of Health (NIH) and Centers for

Disease Control and Prevention (CDC) have also played

a role in the response to the epidemic. For its part, FDA

has issued 10 emergency use authorizations (EUAs) for

products to treat or diagnose Ebola. The agency has also

granted orphan designation to many products in

development to treat Ebola, and says it has deployed "at

least 12 FDA employees … to West Africa as part of the

Public Health Service's team."

Guidance: FDA says its new draft guidance,

Recommendations for Assessment of Blood Donor

Suitability, Donor Deferral and Blood Product

Management in Response to Ebola Virus, is intended to

be used when there is an ongoing Ebola outbreak with

"widespread transmission in at least one country.

"While Ebola symptoms typically present within 21 days

of infection, recent analyses have demonstrated that

some patients may not become symptomatic till much

later. Additionally, scientists have discovered that

infectious Ebola virus and viral RNA can remain present

in certain parts of the body and bodily fluids for months

after symptoms have resolved. Other reports have

signaled the possibility of asymptomatic infection, which

could in theory lead to infection of others.

For these reasons, FDA is recommending blood

establishments implement additional screening

measures when the CDC declares there is widespread

Ebola transmission in one or more countries. Facilities

that collect blood or blood components are instructed to

ask potential donors about any history of Ebola infection,

travel or residence in any country effected by an

outbreak or contact with infected persons in the previous

eight weeks. FDA says that blood establishments should

indefinitely defer donors who have had Ebola virus. The

agency also recommends deferring donation by eight

weeks for any donors who traveled to or lived in an

effected country, or were in close contact with an infected

individual.

The guidance goes on to advise blood establishments on

what actions to take in case blood is collected from an at-

risk or infected donor, including instructions on sample

destruction and when to report a biological product

deviation (BPD) to FDA.

Convalescent Plasma: WHO has identif ied

convalescent plasma, or plasma gathered from

recovered Ebola patients, as a potential treatment for the

disease. While some uncontrolled studies have been

conducted to investigate the use of convalescent plasma

to treat Ebola, such uses are still considered

investigational by FDA and WHO. Thus, FDA says that

any establishments that intend to "collect or distribute

convalescent plasma intended for transfusion in the

United States must submit an investigational new drug

application." Similarly, device sponsors are expected to

follow investigational device regulations for any new

device to be used for such purposes.

Courtesy : Regulatory Affairs Professionals Society

(RAPS)

Molecule clears Alzheimer's plaques in

mice

A molecule can clear Alzheimer's plaques from the

brains of mice and improve learning and memory,

Korean scientists have found in early tests.

Exactly how it gets rid of the abnormal build-up is not

understood. The small Nature Communications study

hints at a way to tackle the disease even once its in full

swing, dementia experts say. But there is no proof the

same method would work in people - many more years of

animal trials are needed first.

Plaque-busting

Currently, there is no cure for Alzheimer's disease.

Treatments can lessen the symptoms, but scientists are

looking for ways to prevent, halt or reverse the disease.

As the dementia progresses, more plaques (clumps of

Technical News


abnormal proteins and chemicals) form in the brain and

healthy brain cells die off. Scientist’s reason that

preventing or removing the plaques might help, and

many drug candidates are in development.

Some drugs still being tested appear to stop the plaques

from forming - but that is if it taken early enough, before

the disease has advanced. However, the South Korean

researchers believe they may have found a molecule,

called EPPS, that could work even if plaques have

already formed. They gave EPPS to mice (bred to have

the Alzheimer's plaques) by spiking their drinking water

for two weeks, and then monitored them over the next

three months to see what effect it might have.

Compared with a control group of mice who received

only normal water, the EPPS mice performed better on

memory and learning problems (running through a

maze). The EPPS mice also had far fewer plaques in

their brain at the end of the trial than they had had at the

beginning. The same could not be said for the control

group.

The Alzheimer's Society and Alzheimer's Research UK

said it was important to remain cautious - animal study

findings may never apply to humans.

Prof Tom Dening, an expert in dementia research at the

University of Nottingham, said: "From a clinician's point

of view, this research is of interest, but we still don't know

if removing amyloid plaques is useful in humans.

"It may well be that the appearance of plaques is too far

down the chain of molecular processes to be beneficial.

"We don't know if this animal work will lead to any useful

agent that can be used for clinical trials."

Courtesy: BBC News

Ready or Not, Aptamers Have Arrived

Aptamers (from the Latin aptus meaning “fit” and the

Greek meros meaning “part”) or “part that fits” are a

relatively new arrival on the food safety testing scene,

demonstrating immediate potential to significantly

change our capability in isolating and interrogating

bacteria and viruses.

Aptamers are amino acid molecules that are synthesized

in high volumes by polymerase chain reaction (PCR).

Functionally, aptamers that are formatted in assays

perform the familiar “lock & key” binding to either proteins

or chemical molecules, and the results of this binding

reaction then enables the detection of the material

(protein or chemical) of interest.

Aptamers may also be used to “capture” and concentrate

bacteria or virus within a sample. The implications of

using aptamers in sample concentration are increased

sensitivity and specificity of assays with lower detection

limits. Aptamers conjugated to magnetic beads may be

used to isolate bacteria or virus in samples.

The methods used to develop and manufacture

aptamers provide significant advantages in reagent

performance. Aptamers can be “fine tuned” by repetitive

rounds of increasingly specific physical structure

refinement of their amino acid sequence to meet

challenging applications. Because aptamers are

manufactured with precision by chemical reactions, their

use in assays eliminates the concern of lot-to-lot

variations in performance.

The Lost Decades of Aptamers

For almost two decades, the scientific exploration and

development of aptamers as important reagents has

been constrained by patent protections associated with

the science of their creation by an iterative process

known as “Selex.” Until recently, other than the work of

the Selex patent holder, development work with

aptamers has been mostly limited to producing reagents

and diagnostic assays for government, homeland

security, NASA and military use.

Beyond food safety testing, aptamers are now

demonstrating impressive capability in private sector

human heal th d iagnost ics and therapeut ic

applications.With the recent expiration of Selex patents,

aptamers are now being used to develop

commercial/industrial assays, human diagnostic tests

and human therapeutic drugs.

Advantages of Aptamers

Speed: Aptamer-based assays benefit from

sensitivity/specificity that is comparable to PCR

performance and significantly larger aliquot volume

analyzed. This combination of accuracy and sample size

offer the industry unbeatable speed to an accurate

result.

Green & Sustainable: Aptamers are molecules

manufactured from amino acids in a chemical reaction

without the use of any animals or biologics, eliminating

lot-to-lot variations.

Dynamic: Aptamers can be “fine tuned” in the

development process to “optimize” reactivity with the

target protein or chemical. This process of optimizing the

aptamer assures that, for example, a Listeria assay does

actually detect the entire Listeria genus. Another benefit

of fine tuning is the ability to distinguish viable from

nonviable (living vs. dead) virus.


Flexible: Several formats for aptamer-based assays

have been developed to meet the needs of a diverse

testing community. In addition to familiar lateral flow

testing devices, 96-well plates and fluorescent digital

readers are available to meet the needs of the end-user.

Costs: Aptamers have a very low cost to manufacture

after the aptamer sequences are characterized and the

assays are formatted and validated. The cost advantage

of not using animals in the production of reagents is a

positive step in economics, and reagent purity and

sustainability.

Future Implications

In addition to enhanced capability in current testing for

pathogens, the implications of aptamer-based assays

include potentially significant enhancement in rapid,

digital quantitative analysis for indicator organisms that

include MPN for generic Escherichia coli and coliforms,

Staphylococcus and total aerobic bacteria counts.

Aptamer methods currently in development for

pathogens detection have demonstrated significant

performance benefits in speed to results. Aptamer

assays have the potential to shorten enrichment times by

up to 50% or more.

Courtesy : FSM E Digest

Good Laboratory Practice for the Quality

Assurance of the Measurement Process

Quality Assurance of the Measurement Process means

establishing, documenting, implementing, and

maintaining a quality system appropriate to the

laboratory’s scope of activities. Having such a system in

place will allow the laboratory to know, within the limits of

a measurement process, that a measurement is valid

with respect to its traceability, accuracy, and precision.

The validity of tests and calibrations should be monitored

with quality control procedures. Statistical techniques

are used to record and monitor charted measurement

results to permit the detection of trends. The metrologists

and laboratory management should plan and review the

results from quality assurance monitoring.

Other steps taken to ensure the quality of the

measurement process may include, but are not limited

to:

• the regular use of Standard Reference Materials

(SRMs) and /or internal quality control using secondary

reference materials;

• participation in interlaboratory comparisons (round

robins);

• test replications with same and/or different methods;

• recalibration of retained items;

• correlation of different characteristics of an item; and

• proper calibration intervals.

Each measurement parameter in the laboratory’s scope

of activities must be reviewed and analyzed to determine

the validity of the measurement process.

The standards and the measurement process for each

parameter must be in a state of statistical control.

Statistical control means that the variability of the

measurement process is known and stable; when a

process is in statistical control, we can assume that the

reported measurement uncertainties are valid. The

National Institute of Standards and Technology provides

technical guidance and support to laboratories to

develop suitable measurement control programs that

provide measurement assurance. The objective of these

programs is to evaluate the entire measurement process

including:

• procedures;

• standards;

• equipment;

• personnel; and

• environment.

While other quality assurance programs could meet

these objectives, the control programs developed for

measurement assurance greatly increase the

comprehensiveness of the program.

State weights and measures laboratories typically

provide measurement services in the disciplines of

mass, volume, and length. Some of the weights and

measures laboratories provide services in other

measurement areas. Approximately 89 % of their

workload is in mass standards calibration. Mass

calibration is the first discipline for which a measurement

assurance program was developed in the 1960’s and

was implemented in State laboratories in the 1980’s.

Nevertheless, all measurement disciplines must have a

measurement assurance system in place.

The most recent improvement in assuring the quality of

each measurement parameter in the State Laboratories

is the incorporation of a Process Measurement

Assurance Program (PMAP).

The PMAP system consists of duplicating the

measurement process by including a check/control

standard as surrogate for the test item. Measurements

made over an extended period of time, typically at least a

year, will show all the conditions that are likely to affect


the measurement process and their combined effects.

Controlled duplication of the measurement process

provides for the realistic evaluation of the measurement

variability as one of the primary components in the

estimation of the measurement uncertainty.

Measurement results that are collected over several

years may be statistically evaluated with current results

being compared to results from previous years. Any

observed problems or changes in the measurement

results are investigated and if necessary, corrective

action can be taken. Ongoing monitoring establishes a

continuous, comprehensive, internal measurement

assurance program in the laboratory.

Data from internal measurement assurance programs

may be compared to the results of interlaboratory

comparisons (round robins) or proficiency tests in which

the laboratory participates.

The strength of the measurement assurance approach

lies in its applicability to a wide variety of measurements

with sufficient flexibility to permit each measurement

control program to be tailored to the particular needs of a

given measurement area. The sophistication of the

control program depends on the criticality of the

measurement.

Courtesy: www.nist.gov

Good Laboratory Practices and Safety

Assessments

Having confidence in scientific procedures and data is

the sine qua non for determining the safety of chemicals

and chemical products. For decisions of safety, there

must be rigorous and thorough application of

fundamental scientific practices, irrespective of the

p u r p o s e o f t h e s t u d y a n d w h e r e i t i s

conducted—academic, industry, or a contract laboratory.

Investigations must be designed and conducted by

experts; whenever possible, standardized and validated

test methods and test systems should be used, test

devices and instruments must be appropriately

calibrated and their accuracy assured, and, most

important, all of the data, including raw laboratory

records, should be available for independent review.

Good Laboratory Practice (GLP) requirements, based

on these fundamental scientific principles and practices,

are indispensable for providing scientific confidence in

studies conducted for chemical safety determinations.

These reasons explain why government agencies

worldwide require GLP compliance, and why it is entirely

appropriate for greater weight to be given to GLP studies

than non-GLP studies that are only available as articles

in scientific journals. In their commentary Myers et al.

(2009) argued that noncompliance with GLP should not

be used as the sole criterion for excluding studies from

consideration in regulatory decision-making. We agree

that GLP should not be the sole criterion, but we

s t r e n u o u s l y d i s a g r e e w i t h t h e a u t h o r s ’

mischaracterization of the purpose and function of GLP

and with their conclusion that GLP has no utility for

weighting the reliability of studies.

Evaluating the safety of any substance should include

review of all relevant studies utilizing a systematic

weight-of-evidence framework. Although not all studies

that are useful for hazard characterization and risk

assessment may be amenable to GLP (e.g.,

epidemiology and mechanistic studies, studies

conducted before the acceptance of current GLP), this

does not obviate their consideration. Each study, GLP

and non-GLP, should be evaluated and weighed in

accordance with fundamental scientific principles.

Factors to be evaluated include

a) verification of measurement methods and data;

b) control of experimental variables that could affect

measurements;

c) corroboration among studies;

d) power (both statistical and biological);

e) universality of the effects in validated test systems

using relevant animal strains and appropriate

routes of exposure;

f) biological plausibility of results; and

g) uniformity among substances with similar attributes

and effects.

Regulatory agencies [Food and Drug Administration

(FDA) and U. S. Environmental Protection Agency

(EPA)] and the National Toxicology Program (NTP)

require studies to be conducted in accordance with GLP

(FDA 2005; NTP 2006; U.S. EPA 2007a, 2007b), and the

Organisation for Economic Co-operation and

Development (OECD) GLP principles (OECD 1998)

apply to all OECD member countries.

Academic basic research is very different from

regulatory research and testing. Academic research

focuses on developing and evaluating new hypotheses,

on creating novel methods, and on discovering new

findings. Academic research is open to wide

interpretation and may require significant additional

studies to clarify and determine whether and how

broadly the results apply. Although novel techniques and

discoveries of academic investigations stimulate further

research, they must also stand up to the scientific

method: hypothesis formulation, hypothesis testing, and



validation by independent replication. Independent

replication provides critical information on the strength of

the hypothesis and reliability of test methods.

Inconsistent results can arise from use of novel

techniques, different test systems, uncertainty and

differences in test chemical composition and purity, and

a myriad of other factors. These facts, in conjunction with

the more limited availability of actual data in most journal

publications, means regulatory agencies can face

significant challenges in confirming the quality,

performance, or data integrity of results obtained solely

from information available from a typical article in peer-

reviewed journals. Whereas all study records and data

from GLP investigations are available to agencies,

rarely, if ever, are such details made available as part of

the peer-review process for publishing a manuscript in a

scientific journal. This can limit the ability of an agency to

independently evaluate conclusions or to conduct

alternative analyses of the data. The challenges faced by

the peer-review procedures of journals have been

recently highlighted (Nature 2006), and it has been

pointed out that “…scientists understand that peer

review per se provides only a minimal assurance of

quality, and that the public conception of peer review as a

stamp of authentication is far from the truth” (Jennings

2006). Journal peer review relies on summarization of

experimental procedures and results, and does not

include examination of laboratory study records or raw

data. The purpose for journal peer review is to judge

whether the study has been conducted and reported

according to internationally recognized, general

scientific standards and whether the study meets the

interest level for dissemination to scientific community. It

is not designed to provide assurance of accuracy or to

recalculate raw data, and it does not provide an

opportunity for independent audit of the study. Myers et

al. (2009) failed to clearly make these distinctions.

Relevant internationally agreed test methods are used

by industry to generate toxicity data for safety

determinations by regulatory agencies. Incorporation of

GLP in these laboratory tests assures that written

protocols and standard operating procedures for each

study component are developed and carefully and

completely followed. GLP also requires meticulous

adherence to dosing techniques; the use of adequate

group sizes to allow meaningful statistical analysis;

characterization (identity, purity, concentration) of test

and control substances, including dosing solutions;

detailed recording of study measurements and data; and

collection of all raw laboratory data in a manner that can

be retained and made available for regulatory agencies

to audit and reach independent conclusions. Quality

control procedures, quality assurance reviews, and

facility inspections are also used to monitor and enforce

GLP compliance. The relevance, reliability, sensitivity,

and specificity of most test methods required of industry

by regulatory agencies are well understood because

they have been subjected to extensive, round-robin

validation programs conducted in numerous laboratories

throughout the world. This high level of scientific rigor, in

conjunction with the detailed processes of GLP, provides

regulatory agencies increased confidence in both the

relevance and quality of GLP scientific studies for safety

decisions, and it is the reason it is wholly appropriate in

regulatory decision making for greater weight and

confidence to be afforded to studies conducted in

accordance with GLP.

Courtesy: Environ Health Perspectives

f. Enrolment in good EQAS / PT programs .

g. Regular review of internal QC and EQAS data.

I have tried to discuss each of these in some detail in the next few paragraphs.

a. Setting and understanding quality goals and types of errors

The QC team first needs to clearly understand the level of quality needed for a particular analyte and set quality goals and how much total error is allowable for an assay. It is only then can the QC protocol for an analyte be defined.The lab staff should have a good understanding of the QC system- something we find largely lacking most of the times. They should be able to judge different types of error, the causes of those errors and should be adept at troubleshooting. They must differentiate between random errors and systematic errors and understand common causes of both, such as specimen problems, electrical issues, mechanical issues with instruments as causes of random errors and reagent problems and calibration issues for systematic error.

A documented training program is the only way that this can be ensured. Staff must be encourage to handover details on on going QC issues to each other between shifts .

b. QC materials are of paramount importance:No amount of emphasis can be too much, when it comes to the use of good reliable QC materials by the lab and their correct handling. Freeze dried and liquid stabilised materials are the two basic kinds of QC materials that are available to laboratories. Storage and use according to the manufacturer’s instructions is crucial to QC performance and should be emphasised to staff. Some

Quality Control systems in medical laboratoriesLet us get a grip on them.

Dr Puneeta Bhatia, MD

The quality management system is undeniably the backbone of any medical diagnostic laboratory. It is comprised of many processes that work together in unison to provide reliable and accurate reports to patients. Amongst these, the quality control system (commonly referred to as QC) in any laboratory has an extremely vital role.

An effective QC system not only ensures that medically significant errors are picked up on time; it also looks into the fact that the lab does not have false rejections. False rejections imply unnecessary repeats which in turn lead to increased cost, waste of reagents, labour, wear and tear of instruments and delayed turnaround times.

There is a difference between establishing a proper QC system and simply doing a set of uncoordinated activities. Any good, robust QC system must be well understood by all laboratory staff, needs to be documented adequately, must be implemented correctly and last but not the least, and is subject to regular analysis, audit and review.

A study of results from a Q – probe survey of over 500 institutions in the USA was published in a paper titled “clinical laboratory quality control: a costly process out of control “(1). The study found that quality control processes were complex and highly variable among participant labs and often differed from established quality guidelines. It concluded that QC is a costly process and laboratory physicians , often do not follow established QC processes, partly because they are complex and often not well understood by the team .

The authors suggested that QC practices must be simplified in order to improve compliance.

A good Quality control system ought to have several features:a. An understanding of analytical error and the types of

errors that can occur in the testing system.

b. A good understanding of the kinds of errors seen in day to day QC practices .

c. The availability of good and reliable QC materials

d. QC rules that the lab will follow to accept / reject the analytical run

e. A process that is followed when the QC values are out of control


Dr. Puneeta Bhatia is a medical laboratory professional with 15 years of experience. She has done her MD in Biochemistry and is a Lead and Technical Assessor for NABL. She also holds an executive management diploma from the IIM, Kolkata. She has worked with reputed organizations like Columbia Asia Hospitals, M.S Ramaiah Medical College and Quest Diagnostics. Her areas of interest include quality assurance in health care, inborn errors of metabolism and prenatal testing.

to typographical errors or due to interchange of QC levels) or else we may not get a correct idea of true variation in the assay.

f. External quality assurance / Proficiency testing programs:

External quality assurance is a vital aspect of the QC system of a laboratory. EQAS programs help to certify that the results produced by the lab are fit for clinical use and are consistent with results being reported by peer labs. The laboratory is able to gauge the accuracy of its results using EQAS.

ISO :17043 accreditation for PT providers has further ensured that the EQAS programs available are compliant with international standards that have been developed for this purpose.

The end of cycle report furnished by most EQAS programs provides tremendous insights and learning to the laboratory with details of each parameter- such as imprecision, relative rankings, bias from method mean, bias from peer group mean and trend analysis to name just a few .

g. Integrated assessment of IQC and EQAS dataIntegrating inputs from Internal QC data and External quality assurance reports is the key to a establishing a robust QC system. The quality analyst should be capable of integrating the two sets of information from IQC and EQAS and making changes to calibrations, correction factors after a holistic based upon both sets of data .

h. Use of patient data for QC :Another approach is to use patient data to keep a track on the analytical quality. An important advantage of this is that there is no matrix effect , unlike that with synthetic QC sera. Trends in patient values, bizzare results that are incompatible with life, patient sample duplicate runs, retained sample testing are all valuable inputs obtained from this practice.

A quality control system that rests on all the above pillars is quite likely to pick up most laboratory errors in the analytical phase and would decidedly go a long way in providing accurate and reliable results to our patients.

References: 1. T. Badrick, The Quality Control System, Clin

Biochem Rev Vol 29 Suppl (i) August 2008 , S 67- S 70 .

2. Burtis, Ashwood , Bruns , Tietz Textbook of Clinical

Chemistry & Molecular Diagnostics, 5 th edition .

analytes may be unstable upon thawing or upon reconstitution. These can be sources of major error if not tested within time limits defined by manufacturers. It should be ensured that the QC material covers the range of clinical interest of each analyte .

c. Using QC rules judiciously QC rules, better referred to as statistical process control ( SPC ) rules help us interpret the results of QC runs. There are various rules available but they all have their limitations .No rule will detect all the error that is present and sometimes the rules used will falsely suggest errors in the system. A common practice is to use a set of rules, commonly called multi- rules , applying them in sequence to increase the sensitivity of error detection at a particular false rejection level. The most commonly used set of multi rules are the Westgard multi rules. Plotting the QC data in the form of Levey Jennings charts, cusum charts, power function graphs and many more such tools is a good practice for any laboratory. These graphical tools tell us much more than the numbers. A good glance at the day’s charts is enough to tell an experienced eye that the systems are in control.

d. Corrective action for QC failures :It is critical for medical technologists to know what is to be done in the event of a QC failure or outlier. The commonest response is to repeat the QC run or recalibrate the assay, both of which are not the wisest of things to do without adequate introspection into the cause of QC failure. One approach would be for the laboratory to implement an SOP or an algorithm that needs to be followed by technologists in the event of QC failures.

Documentation of QC failures must be diligently done on a real time basis, corrective action taken and patient impact, if any, must be noted. This data should be reviewed regularly, for it has many a lesson to teach the discerning mind.

e. QC statistics for the laboratory:All QC systems that involve the use of synthetic QC sera require that the mean and SD be set for all analytes being run on that system . These statistics correctly reflect the repeatability and reproducibility of the assay from one run to another. This requires mean and SD to be determined over a reasonable number of analytical runs. This does add to cost undoubtedly, but then it helps to put in place a robust QC system which in turn leads to less repeats, better patient results and more customer satisfaction. Running different QC material over as many different runs as possible also helps to identify variation from one vial to another or changes due to thawing or due to reconstitution. Failed QC data ought to be included in the calculation of mean and SD (with the exception of bizarre values that may have occurred due


Recent Trends in analysis of Vitamins

Dr BalasubramanianHead Techncial

Chennai Mettex Lab Pvt Ltd.

Vitamins are a class of organic compounds categorized

as essential nutrients. They are required by the body in

very small amounts. They fall in the category of

micronutrients. Vitamins are divided in to two groups: fat

soluble vitamins- A, D, E and K and water soluble

vitamins: vitamins of the B-group and vitamin C.

One of the major upcoming issues is increasingly tough

legislation being enacted or being discussed for

regulatory compliance in fortified food products. The

introduction of stricter regulatory compliance places

even more importance on the need for well-validated

internationally accepted analytical methods of high

precision.

Analytical methods in general must be reliable and

robust to be useful. The analyte must be stable during

the analytical process, both extraction and

chromatographic procedure must be reproducible, the

results should be accurate and the uncertainty should be

small. The detector should be selective for the analytes

of interest. The analyte of interest should be free from

matrix interferences and the method should be free from

matrix effects.

For Example, Vitamin B12 is fortified 10-20 µg/100g level

in nutritional food products. Microbiological method of

Vitamin B12 is replaced with immune affinity column

separation technique in nutritional food products. The

new method Developed by using Immuno affinity column

is extracted and quantified using AOAC 2011.08 method

is showing good recovery and precision at low levels

using HPLC.

The discussion of methods for individual vitamins will

emphasize the handling and preparation of samples for

analysis; these are crucial factors because of the liability

of some vitamins. Many vitamins are sensitive to light

and some can be oxidized very rapidly. Heating can

increase the rate of oxidation and may also lead to

isomerization to inactive forms; unnecessary heating

should therefore be avoided.

Bottlenecks in Vitamin analysis:

? Most of the vitamins are sensitive to light.

? Single vitamin is in different bound form (Thiamine is


in two forms-thiamin hydrochloride & thiamin

mononitrate)

? Some of the vitamins required specif ic

derivatization.

? Heating should be at idle temperature.

? Some vitamins can be analyzed both in normal and

reverse phase form.

? Form of fortification plays a major role in choosing

method.

? Selection of method will vary based on the

commodity.

? Each Vitamins has to analyzed alone to get the

better results.

AOAC INTERNATIONAL has formed an AOAC

Stakeholder Panel on Infant Formula and Adult

Nutritionals (SPIFAN). Current funding for this effort is

made available through the Infant Nutrition Council of

America (INCA), formerly the International Formula

Council (IFC). This panel has been established to

develop standard method performance requirements

(SMPR) for priority nutrients in infant formula and adult

nutritionals. Since April 2010, 28 SMPRs were

completed and adopted as standards along with 43 First

Action Official MethodSM adopted. SPIFAN II was

signed in mid-June 2013, to continue the focus on

completing the nutrient panel through September 2016.

In August 2013, AOAC launched biotin, FOS/GOS,

vitamin K, and minerals. The next sets of nutrients to be

launched are amino acids, carotenoids, fluoride, and

chloride in March 2014. The final sets of nutrients to be

launched in September 2014 are vitamins B1, B2 , B3,

and B6. For each nutrient, a working group is formed for

the purpose of developing the standard method

performance requirements. An AOAC Expert Review

Panels will approve one method as First Action Official

MethodSM that will eventually undergo multi-laboratory

testing (MLT) in support of achieving Final Action Official

MethodSM status. SPIFAN is continuously seeking

qualified laboratories to participate in these MLT studies.


Summary:

Food industry requires simple and more rapid QC

procedure for Vitamins (Fat & Water Soluble Vitamins).

Methods have to be developed based on the commodity

and very few methods can be used to extract the

vitamins entire commodity. Recently Immunoassay kits

for Vitamin A and D in milk and dairy products are

available. Initial trials show that these procedures

Notes: GC = gas chromatography; HPLC = high-performance liquid chromatography; UPLC: Ultra performance liquid Chromatography;

require some further optimization to render them

sufficiently robust for routine analysis.

In future commodity specific method is required to get

the better performance and valid analytical data and the

studies are going on in to develop robust method.

The above mentioned AOAC Methods will be published

in ISO very soon, and will be available as International

methods for the analytical communities across the world.

Is lab testing the 'Wild West' of medicine?

Descending in darkness, a FedEx Corp. cargo jet

touched down on a runway, at Rochester, at 5:44 a.m.,

filled with hundreds of identical, raspberry-colored

boxes.

A truck painted the same color soon sped the boxes, all

human blood and cell samples, to more than 40

laboratories at the nearby Mayo Clinic, based here. Most

every day, an onslaught of about 30,000 specimens

arrives for tests to answer what can be life-or-death

questions: Does the patient have cancer? Which drug

treatment has the best chance of success?

The predawn drill is part of the multibillion-dollar-a-year

business in “lab-developed tests.” An estimated 100,000

such tests have been developed by hospitals and lab

operators, which screen samples sent by doctors, other

hospitals and consumers. That differs from traditional lab

tests, where companies sell diagnostic machines and

test kits for use across the U.S.

The Food and Drug Administration sees lab-developed

tests as the Wild West of medicine, citing examples of

inaccurate tests it claims put patients at risk. The agency

is trying to toughen its supervision next year after largely

leaving the business alone for decades and focusing

most of its oversight on traditional testing methods.

Lab-developed test providers are fighting back. They say

their tests are accurate and even lifesaving. Industry

officials say heightened regulation could stifle

innovation.

Courtesy: Wall Street Journal

Projections of Global Food safety market:

The global food safety testing market is projected to

reach a value of USD 16.1 Billion by 2020, at a CAGR of

7.4% from 2015.

The global food safety testing market has been showing

dynamic growth with the increasing concerns for food

contamination and foodborne illnesses. The market has

been experiencing growth, driven by increasing

consumer awareness related to food safety issues. All

regions have experienced severe outbreaks of

foodborne illnesses and toxicity cases. Worldwide,

stringent food safety regulations have been

implemented to restrict the presence of pathogens or

chemical contaminants that are responsible for the

outbreak of foodborne illnesses. The market includes

food testing laboratories as well as technology providers.

These market players are experiencing increasing

demand for food safety testing due to the concern of

product recalls from food manufacturers and health

issues from consumers.

North America dominates the global food safety testing

market. The North American food safety testing market

has expanded due to the increase in the number of

foodborne disease outbreaks and food contamination.

Canadian regulations are the most stringent and strongly

support the food safety testing market. It has been

observed that this country has emphasized widely on the

inspection of imported food to judge the quality and

safety of the food.

The number of in-house testing laboratories in North

America has doubled, with the aim to protect the quality

of the product. Outsourcing food safety testing has

benefited food producers in cutting down costs, and has

encouraged the growth of this market. Recognized

testing laboratories have increased the reputation of a

company’s food quality.

In Europe, food safety policy has been emphasized by

the contributed efforts from Control Laboratories (CLs),

National Reference Laboratories (NRLs), and EU

Reference Laboratories (EURLs). These authorities

have a vital aim of protecting consumer health by

assuring the quality of the food supply chain. Food safety

policies integrated in Europe follow the strategy of "from

farm to fork."

The Asia-Pacific region is the fastest-growing for the

food safety testing market due to consumer awareness,

regulatory bodies, and manufacturers taking necessary

steps to avoid food product contaminations and product

recalls. The growth has been majorly driven by the

Chinese food safety testing market, as they have

increased emphasis on food security dwelling internal

and external to China.

The spread of food safety information has been

encouraged by the availability of new testing

technologies. Consumers and regulatory bodies are

scrutinizing food firms to provide more information about

pathogens in their products. This has assisted in setting

food safety regulations and developing specificity of

demand. The protection of domestic consumer health

and assurance of exported food safety and quality have

been approved by the National Food Control System.

Though food safety has shown alarming signs across the

world, some countries have been negligent on testing

food for contaminants. In this case, governments need to

take vital steps to set food safety testing mechanisms.

Trade News


Nevertheless, this situation will be tackled by the ever-

growing efforts of regulations, companies, and partners

of food safety systems. The global food safety testing

market has been dominated by meat and poultry

products owing to the fact that maximum number of

illnesses are attributed to them. Rapid food safety testing

technology dominated the market in 2014.

The figure above depicts the global market size of food

safety testing market by region. The North American

market is estimated to hold a major share in 2015.

The global food safety testing market is projected to

reach a value of USD 16.1 Billion by 2020, at a CAGR of

7.4% from 2015.

Courtesy: Markets and Markets

Faster, Better, Cheaper… What’s Most

Important in a Pathogen Test?

For close to 20 years, Strategic Consulting (SCI) has

been following the industrial microbiology market, and

food safety testing applications in particular. As part of

the data gathering for our most recent report, Industrial

Microbiology Market Review, SCI interviewed 15 senior

managers at major food companies and food contract

labs (FCLs) to understand their priorities when choosing

a pathogen diagnostic method. The interviews were

roughly split between food companies and food contract

labs.

SCI identified 10 important attributes for evaluating a

diagnostic method or instrument, and asked the

interviewees to stack rank the top five items most

important to them.

The three top-ranked choices were the same at both

food companies and FCLs, with sensitivity/specificity the

most important attribute. Second in importance was the

ability of the method to be utilized in a broad range of

food matrices. Ranking third was the cost per test for

diagnostic reagents.

For food companies, time to results (TTR) was tied for

third in the stack ranking, followed by ease of use

(EOU)/automation in fifth place. Clearly, food companies

want quick results but only after they are assured that the

pathogen diagnostic they are using provides accurate

results and is able to work with a range of food types.

For food contract labs, the cost of the pathogen

diagnostic instrument ranks fourth, and TTR is tied with

the cost of labor per test for fifth. For FCLs, most of the

key attributes in method selection are based on

operational considerations, which makes perfect sense

given testing is their business.

Courtesy: FSM E Digest

Odisha seeks two food testing labs

The state government has sent a proposal to the Union

ministry of food processing industries (MoFPI) for

establishing two food testing laboratories in the state to

give a boost to the processed food sector.

The directorate of export promotion and marketing


(DEPM), Odisha has prepared an initial project report,

containing scope of testing items and list of machines

needed for the two labs to be set up at Cuttack and

Berhampur. The new centres will be housed at the

testing facilities of DEPM at Cuttack and Berhampur. The

cost of the two labs is estimated at Rs 7.37 crore.

The testing to be done at the two centres are milk powder

and skimmed milk powder, Indian curry powder, wheat

atta, biscuits, carbonated drinks, honey and black

pepper among others.

DEPM has six testing labs located at Cuttack, Bolangir,

Balasore, Angul, Berhampur and Rourkela. However,

none of the testing centres have the facilities to test the

processed food items. Sources said, as many as 32 food

processing industries in the state have gone into

production in 2014-15 financed under the National

Mission on Food Processing.

"The proposed food testing labs at Cuttack and

Berhampur is pivotal as the state government has

already put in place an Odisha Food Processing Policy-

2013. The testing facilities will also encourage


entrepreneurship in the food processing sector," said a

DEPM official. In addition, the processed food

manufacturers do not have to travel to other states for

getting their products tested, he added.

Officials said, the testing centres assume significance as

the state government is in the process of setting up of

more food parks in the state. Recently, the state

government has decided to set up 20 new agro/food

processing parks.

Odisha Industrial Infrastructure Development

Corporation (Idco) was asked to prepare techno-

feasibility report for 15 mega food parks. The Odisha

Small Industries Corporation (OSIC) will undertake the

task for five parks.

The MITS mega food park is in the process of

implementation in Rayagada district while the Huma

Mega Coastal Food Park in Ganjam district, which was to

be developed under the Mega Food Parks Scheme was

rejected by the Centre recently.

Courtesy: Business Standard

BASICS OF INTERNAL AUDITDevi Saran Tewari

Chairman - AOIL

The criteria for laboratory accreditation, ISO/IEC 17025

(2005), the International Standard for Testing and

Calibration Laboratories may undergo a change from

time to time but the concepts on its various clauses

including on internal audit would remain the same.

Audit would loss its meaning if it is without impartiality,

and to ensure impartiality, one has to abide by the conflict

of interest and to the principle of independence for

auditor and for all type of audits, be it external audit or the

internal audit.

The moment audit is taken as a tool to determine the

effectiveness of the implementation of the management

system by management itself, it becomes a means for

self-improvement for that establishment, and it is called

internal audit. Those managements who opt for it, find it

useful as this leads to detect the slips and also in

preventing the wrong from happening. This also

provides the chance to take corrective measures and to

control the damage.

The modern concept to include the conduct of internal

audit as a part of management system in all most all

standards makes it a mandatory requirement, is the

recognition of the role it plays to ensure the quality for the

desired objective. In the case of Test and Calibration

Laboratories it has been accomplished by including a

clause for Internal audit in ISO/IEC 17025, the

international standard.

ISO/IEC 17025: 2005, has been written in such a that for

several critical requirements it expanse how the

requirement should be achieved. If clause 4.14 requires

the conduct of internal audit then clause 4.1.5 f, gives the

directive on how to abide by it and ensure that its

management system is effectively followed and

implemented.

4.1.5 (f) says “ laboratory shall appoint a member of staff

as a quality manager ( however named) who,

irrespective of other duties and responsibilities , shall

have defined responsibilities and authority for ensuring

that the management system related to quality is

implemented and followed at all times; the quality

manager shall have direct access to the highest level of

management at which decision are made on laboratory

policy and resources.

Let us understand what it says;


i. Appoint a member of staff as quality manager,

irrespective of other responsibilities….., It implies

that internal audit is an internal activity which has to

be completed labs staff.

ii. Define responsibilities and authority for ensuring

that management system related to quality is

implemented and followed at all times; Implies that

by Conducting internal audit, Quality manager

determines, if the management system is being

implemented, and when, Quality manager, verifies

for completion of corrective action for the NCs

found, it is to ensure that management system is

followed for all times.

iii. The directive that Quality manager shall have

access to highest of management is meant to

ensure the Independence to quality manager to

conduct his work.

iv. To retain impartiality in the conduct of internal audit,

one has to refrain from doing the audit of his own

work.

When clause 4.1.5 f directs that laboratory shall appoint

a member of staff as the quality manager, irrespective

other duties and responsibilities; it needs to respected by

all parties involved.

Respect means if a laboratory does internal audit using

it’s own person, it needs to be taken as the compliance to

clause to 4.1.5 f. On examination of the records of

internal audit, it would be clear if the impartiality was

maintained or not, and for it, one needs to check for

conflict of interest in the conduct of internal audit.

There are cases where laboratories are advised to get

the internal audit done by an out sider, this needs to be

stopped. The reason given for such action is that audit

conducted by internal staff is not independent which

contrary to clause 4.1.5 f.

There is need to develop clarity about the clause 4.1.5 f,

and if required seminars could be organised for healthy

debate.

However, accreditation bodies may define the policy for

one-man laboratory, to abide by impartiality.

Conduct of Internal Audit:

Internal Audit has to be an as impartial activity and

impartiality can be achieved when there is no conflict of


interest. Conflict interest is evident when an auditor does

the audit of his own work. It is not difficult to achieve this

objective except for one-man managed laboratory.

Whether it is internal or external audit, in both the cases

the technique of audit remains the same.

The management of a laboratory is required to assign

the responsibility for conducting internal audit etc. to a

person (Quality manager) who is competent person and

from within the staff of laboratory. The competence of

Quality manager is to be determined based on his

qualification, familiarity with the laboratory working &

documentation, training on conduct of internal audit and

experience.

And to maintain impartiality auditor or the Quality

manager ought to know, to not to audit their own work. In

case of one-man laboratory, audit by the external auditor

is a must and needs to be included in the documentation

of its management system.

The Internal Auditor or the Quality manager has to have

the procedure for conduct of internal audit and he has to

have a plan to conduct the audit. The main components

of the plan are:

i. Schedule of audit.

ii. Checklist of system procedures, etc.

iii. Checklist of technical procedures

iv. Familiarity with other documents like log-sheets etc.

v. Checklist of laboratory personnel

vi. List of work records.

The audit plan has to cover the technique of audit:

i. Horizontal audit

ii. Vertical audit

In the first internal audit of a laboratory, is to be done

against ISO/IEC 17025, to determine if all

procedures/documentation are available. In case of non-

availability of a required procedure/document it needs to

be developed.

It has also to be acknowledged that when a procedure is

followed for a specified job, the work records get

generated. These records are linked to the procedure

followed. And audit is a process of verification of records

against the concerned procedure. Laboratory’s internal

audit is to cover it’s records of work done against the

concerned procedure, and to determine it was followed,

by the concerned person.

In horizontal audit the work records are examined

against the specified procedure of the laboratory, one by

one for each applicable requirement/clause of ISO/IEC

17025.

The formats used to record the audit findings, are meant

to establish that audit was done, against specified

procedure, date, item of audit, person whose work is

being audited etc. When audit against a specific

procedure has been completed then audit finding are to

be brought to the notice of the auditee for seeking

clarifications. In those cases, where auditee is not able to

clarify and agrees for non-compliance, auditor has

confirmed NC. The progress of audit is marked in check

list, one by one till all items for horizontal audit are

completed. Also the checklist of personnel would also be

ticked. When audit is in progress there is no need to

make auditee sit in front of auditor, as it is not required.

Auditor needs only records of the work done for a

specified period and the related procedure etc.

When an NC is noted, it requires seeking time schedule

for completion of corrective action, as auditor has to do

verification for completion corrective action and to

remove NC.

In vertical audit entire scope of the test or calibrations is

covered and one needs to find out the number of jobs test

or calibrations completed for the period to be covered in

the audit. Laboratory auditor has to apply his logic for

picking up the audit samples. The samples drawn for

audit have to be representatives, to justify the audit

which is based on random pick of the sample of audit.

Audit would proceed against each procedure, starting

from receipt of sample, storage condition, sample drawn

for testing, preparation of the sample for testing, actual

testing done, environmental conditions, equipment used

and the traceability, and persons responsible the work at

each stage, data transfer and calculation checking, test

report, authorised signatory etc.

Access to the records/data/ store/archive, for each step

of audit and to check against the procedures are main

component in the vertical audit. One should also

remember the situations where a single person is

responsible to perform the work against more than one

procedure, the audit for his work has to be done against

each procedure.

Verification of corrective actions, compilation and

making a summary for audit reporting, is the last activity

of audit. Before submitting the findings of internal audit to

the management these have to be shared with the

technical manager, with a copy of findings, and also to

abide by the principle of transparency.

Member's PAGEMember's PAGE


comparison or proficiency testing schemes is an

effective way to find out whether the laboratory’s system

is in statistical control.

ILAC Guidelines

ISO/IEC 17011 states that “The accreditation body shall

ensure that its accredited laboratories participate in

PT….and that corrective actions are carried out when

necessary”. This has necessitated the policy framed by

the ILAC to be adopted for Accreditation Bodies/CABs

and the laboratories as well. The ILAC policy says –

“Accreditation Bodies seeking to sign or seeking to

maintain the status as signatory to the IlAC MRA need to

demonstrate the technical competence of their

accredited calibration and testing laboratories. One of

the elements by which accredited calibration and testing

laboratories demonstrate technical competence is by

satisfactory participation in PT activities where such

activities are available”. The ILAC policy also

recommends the minimum appropriate frequency for

participation in PT activities by laboratories – “minimum

on activity prior to gaining accreditation and one activity

relating to each major sub-discipline of a accreditation”.

The shows the importance assigned to the activity of

participation in proficiency testing schemes.

Inter Lab Comparison (ILC)

Participation in collaborative studies is colloquially

referred to as ILC and PT. There is difference in ILC and

PT, an it can be known only in how such schemes are

used. All collaborative studies are termed as inter-

laboratory comparisons. However, when these are used

for evaluating the laboratory’s performance, it is known

as proficiency testing. Detailing the uses of ILC covers

many areas of the laboratory’s functioning

and its control. Some of these include.

1. Evaluation of the performance of laboratories for

specific tests or measurements and monitoring

continuing performance of laboratories.

Introduction

As accredited laboratories play an important role in

liberalizing international trade barriers, their onus is to

produce data or results which can be relied upon and

decisions can be taken without further reference to any

other laboratory. In other words, the customers should

have confidence in results that the laboratory produces.

More so, the laboratory should also have confidence in

the results it produces. It is very difficult and

unmanageable to verify every result. Laboratories Shall

be able to produce repeatable or reproducible results for

every sample tested by it. The question is how it can be

ensured that the results produced in a laboratory by an

operator/analyst for a given sample are repeatable o r

how it can be ensured that the results produced by an

operator/analyst can be reproduced by another

operator/analyst in the same laboratory on the same

sample or how it can be ensured that the results

produced by a laboratory can be reproduced by another

laboratory on the same sample.

Laboratory Competence

The competence of any laboratory can be checked in two

ways – by verifying its competence by assessment of its

operation against some predetermined criteria, or by

participating in collaborative studies like inter-laboratory

comparison (ILC) or proficiency testing (PT) schemes.

The predetermined criteria sought when assessing a

laboratory is usually the international standard ISO/IEC

17025 and ISO 15189. This is done through assessment

by Accreditation Bodies (AB). When a laboratory

participates in collaborative studies, the result obtained

in such studies can give information whether the

laboratory’s system is under control and the results

produced by it can be relied upon. Accreditation is a one-

time activity and regular assessments after accreditation

ensure that the data produced by the accredited

laboratories can be relied upon. In between the

assessments, If the laboratories established system

goes out of control or there seems to be inclination

towards the same, participation in interlaboratory

Inter-LaboratoryComparison & ProficiencyTesting

2. Identification of problems in laboratories and

initiation of actions for improvement which, for

example, may be related to inadequate testing or

measurement procedures, effectiveness of staff

training and supervision or calibration of equipment.

3. Establishment of effectiveness and comparability of

test or measurement methods.

4. Provision of additional confidence to laboratory

customers.

5. Identification or inter-laboratory differences.

6. Education of participating laboratories based on the

outcomes of such comparisons.

7. Validation of uncertainty claims.

8. Evaluation of the performance characteristics of a

method – often described as collaborative trials.

9. Assignment of values to reference materials and

assessment of their suitability for use in specific test

or measurement procedures.

10. Support for statements of the equivalence of

measurements of National Metrology Institutes

through “key comparisons” and supplementary

comparisons conducted on behalf of the

International Bureau of Weights and Measurement

(BIPM) and associated regional metrology

organizations.

Proficiency Testing (PT)

Proficiency testing involves the use of interlaboratory

comparisons for determination of performance of the

laboratory and its testing personnel/analysts/operators,

as listed in 1 to 7 above. Proficiency testing does not

usually address 8, 9 and 10 because the laboratory’s

competence is assumed in these applications. However,

these applications can be used to provide independent

demonstrations of laboratory competence.

Why Should a Laboratory Participate in

Proficiency Testing Scheme

Participation in PT schemes supplements the lab’s QC

programs and provides the evidence of its ability to

produce reliable data. Participation also provides the 4

Cs, viz. comparability, consistency, competence and

confidence for both the lab and its testing personnel.

Comparability and consistency in

laboratory produced data at the international level is

what global trade demands. Competence and

confidence is what the laboratories gain by participating

in the PT schemes. Additionally, the customers of the


laboratory can also have the confidence in the

laboratory’s results. The uses are many. Results

obtained in the PT scheme can be utilized by the

laboratories and their customers, regulatory bodies and

also standard formulation bodies.

There are other benefits in participating in proficiency

testing schemes. Participation in the PT schemes helps

the laboratories in identifying their measurement issues.

In case the result of a PT round is within limits, it gives

evidence to the laboratory that their system is under

control. If the results near the bounds or outside the

bounds, this gives warning or action signals to the

laboratory, which should start taking action accordingly.

The PT canalso be used for comparing methods or

procedures and also for knowing the limits of uncertainty

for a particular test.

Participation in PT schemes also gives information to the

laboratory about the other aspects of the management

system. Besides the testing and analysis, PT also gives

information about sample preparation, data assimilation

and transfer, report generation etc. By participating in PT,

the laboratory can get to know which aspect of its system

is in control and what has started to depart from its set

standards. If under control, PT can be helpful in

improving the procedures and uncertainty in its

measurements. In a nutshell participation in PT is a tool

for

process improvement of the laboratory. The PT also

instills confidence in the laboratory staff.

Most important, participating in PT scheme is a pre and

post accreditation activity. A laboratory needs to follow

the requirements of the accreditation body in relation to

the participation in PT schemes.

Requirements for Proficiency Testing

Schemes

For a laboratory, participation in PT scheme is a way to

know its capability to test a sample using a particular

method. It is required because it is essential for its

accreditation. The laboratory should participate in a PT

scheme which suits its requirements.

Usually, the PT is conducted by PT providers in many

rounds for the same parameter or tests.

For a particular product and test, some three to six

rounds are conducted in a year by the PT provider.

Participation in only one round may give some

information to the laboratory. This may not be enough to

take action for improvement. The result of the PT in a

single round may be due to chance cause. Only after

participating in more PT rounds for the same method,


can the laboratory know about its capability to produce

the results in a consistency manner. Many laboratories

participate in the rounds of the PT schemes to know their

capability. They also have a chance to compare their

result with the results of the other laboratories worldwide.

Apart from the rounds during the year, the laboratory

should also see whether the PT scheme is for tests

covered in its scope of testing. The method of test being

followed in PT should also be that which is followed by

the lab in its normal day-to-day testing. A laboratory

doing chemical analysis of metals should not participate

in a PT scheme for identification of heavy metals in

water, even though it may be capable of the same. The

laboratory should look for PT scheme in the area of its

technical competence, which is usually seen as “one-

product one test one- technique”. A laboratory may have

than more than one area of competence; it may take up

PT in any of the areas. But, in order to cover its entire

scope, it should try participating in many of its core areas

of competence.

The competence of the PT provider is also a very

important factor in the decision for participation in a PT

scheme. The experience of the PT provider and its

competence in planning, conducting and evaluating the

PT scheme shall be looked into. After all, participation in

PT costs a lot of money. Hence a competent PT provider

will only be good value for money. And a competent PT

provider is one which has accreditation as per ISO/IEC

17043:2010 (conformity Assessment: General

requirement for proficiency testing).

Assessment of Lab’s Performance

A proficiency testing scheme involves meticulous

planning and its impeccable execution. A PT provider

does just that. The PT provider is accredited for the

various PTs it is conducting. Its capability to conduct PT

(planning, execution and result) is assessed by the

accreditation body. It prepare samples, assesses its

values (assigned values), conducts PT and evaluates

the results statistically. At the same time, some of the PT

providers educate the participants about their score and

any actions required for improving those scores. In order

to do so, it is essential for the PT provider to establish the

assigned value of the PT test item and the standard

deviation of proficiency testing. Both these statistics are

essential for evaluating the performance of the

participant laboratory.

References

1. Eurachem Guide on Selection, Use and

Interpretation of Proficiency Testing (PT) Schemes,

Second Edition (2011).

2. ISO 13528, Statistical Methods for use of

proficiency testing by inter-laboratory comparisons,

(2005).

3. Anuj Bhatnagar, Measurement & Laboratory

Systems A Comprehensive Guide.

To be completed in next issue….

R.B. Singh,ANULAB, Agra

email:- [email protected]

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