JORDAN FOOD AND DRUG ADMINISTRATION

AMMAN FOOD LABORATORYEdition: 1

Review: 1

Date: 01-10-2017Page 1 of 13

OPERATING LIQUID CHROMATOGRAPHY MASS SPECTROMETER (LC-MS/MS)

No.: AFFsop 10

Content Page

1. Objectives 2

2. Scope 2

3. Responsibility 2

4. References 2

5. Definitions 2

6. Instruments 2

7. Procedure for operating the LC-MS/MS 3

7.1 Start up 3

7.2 Performing Autopurge (LC) 4

7.3 Opening Method File 5

7.4 Acquiring Data 6

7.5 Checking Analysis Results during Data Acquisition (Snapshot) 10

7.6 Quantitative Data Analysis 10

7.7 Shutdown 12Prepared by:Ghaith R. Algharibeh

Date: 1-10-2017

Review by:

Date:

Approved by:Head of

Head of Quality Division

AFFsop 10, Rev 1 Page 1 of 13

OPERATING LIQUID CHROMATOGRAPHY MASS SPECTROMETER (LC-MS/MS)

1. OBJECTIVE

The following document describes the procedure to operate the LCMS-8050-Nexera-i LC-2040c (LC-MS/MS) (Shimadzu-Japan)

2. SCOPE

This procedure applies to the LCMS-8050 set up in the Contaminants Monitoring Division (CMD)

3. RESPONSIBILITIES

It is the responsibility of the CMD staff to follow the instructions & ensure adherence to this procedure

4. REFERENCES

4.1 Getting Started Guide (225-30219 Feb. 2015) (Shimadzu)4.2 Operators Guide (225-30224B Mar. 2016) (Shimadzu) 4.3 Installation & Maintenance Guide (225-30222A May 2016) (Shimadzu)4.4 Nexera-I LC-2040C system guide (2014) (Shimadzu)

5. DEFINITIONS

5.1 MS: Mass spectrometer5.2 LC: Liquid chromatography

6. INSTRUMENTS

6.1 Nexera-i LC-2040c (Ultra Performance Liquid Chromatography) (Shimadzu-Japan)6.2 LCMS-8050 (Mass Spectrometry) (Shimadzu-Japan)

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7. PROCEDURE FOR OPERATING THE LC-MS/MS7.1 Start Up

7.1.1 Please note that the system should always be turned ON7.1.2 Turn ON all of the instruments7.1.3 Confirm that dry air, nitrogen gas and argon gas are being

supplied to the MS instrument7.1.4 Start the PC7.1.5 Verify that the (LabSolutions Service) icon in the system tray

on the Taskbar is green

7.1.6 Double-click on the desktop7.1.7 Log in by pressing (OK)

7.1.8 Click on (LCMS) to start the (Realtime Analysis) program

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7.2 Performing Autopurge (LC)7.2.1 Check mobile phases A & B and rinse solution quantity &

quality7.2.2 Press (Purge) on the LC main analysis screen

7.2.3 Turn ON mobile phase (A), (B) and (Rinse)

7.2.4 Leave the default timing (3minutes for mobile phases and 10 minutes for rinse solutions)

7.2.5 Press (Start)

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7.2.6 After the purge finishes, press (Close)

7.2.7 LC is ready

7.3 Opening Method File7.3.1 In (Realtime Analysis) window, Click on (File) then (Open

method file)7.3.2 Under (Local Disk (C:)) choose (LabSolutions) then (Data) then

(Project1) then (CMD)7.3.3 Choose the required method folder, either (CMD Cereals

(Group 5)), (CMD FV (Groups 1,2,3)) or (CMD Oils (Group 4))7.3.4 Open the required method file (e.g. CMD 180 pesticides

cereals (group5) LC File)7.3.5 Ensure that (Ready) is displayed in the (Data Acquisition)

window

7.3.6 Under (Instrument Parameters View) sub-window, check that the MS, Interface, LC Time Program and Pump parameters are OK

7.3.7 Click (Download) Icon to send method to the instruments

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7.4 Acquiring Data

There are two ways of acquiring data; the first is by single run (only one sample) & the second by real time batch (sequential analysis of multiple samples)

7.4.1 Single Run7.4.1.1 Place the sample in the auto-sampler7.4.1.2 Open the required method file (Section 7.3)7.4.1.3 Click the (Start Single Run) icon under (Acquisition)

assistant bar

7.4.1.4 Set the sample name (Type) (e.g. Cucumber)7.4.1.5 Set the sample ID (Lab report number) (e.g.666-1)7.4.1.6 Set Data File, create into (C:\LabSolutions\Data\

Project1\CMD\Pesticides Results folder)7.4.1.7 Create data file name with sample ID (e.g. 666-1)7.4.1.8 Set the vial # (e.g. 1) & the tray (e.g. 1)7.4.1.9 Set the injection volume (2 µl)7.4.1.10 Make sure that the latest tune file is uploaded (e.g.

26-07-2017 tuning file)7.4.1.11 Set the dilution factor if present7.4.1.12 Set sample amount if present7.4.1.13 Click (OK) & single Run is started

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7.4.2 Real time Batch7.4.2.1 Place the samples in the auto-sampler7.4.2.2 Open the required method file (Section 7.3)7.4.2.3 Click on (Realtime Batch) icon under (Main)

assistant bar

7.4.2.4 Click on (Wizard) icon

7.4.2.5 A wizard sub window will pop up

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7.4.2.6 Set Batch Table to (New)7.4.2.7 Check that the required method file is open (e.g.

CMD 180 pesticides cereals (group5) LC File)7.4.2.8 Set the injection volume (2 µl)7.4.2.9 Set MS Data Processing to (Quantitative)7.4.2.10 Choose (Unknown Only) if running samples,

choose (Standard Only) if starting a standard calibration curve or choose (Standard & Unknown) if standard calibration curve is generated with the samples in the same batch

7.4.2.11 After choosing (Unknown Only), Click (Next)

7.4.2.12 Set the Sample Name (Type) (e.g. Cucumber)

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7.4.2.13 Set the Sample ID (Lab report number) (e.g.666-1)7.4.2.14 Set Data File, create into (C:\LabSolutions\Data\

Project1\CMD\Pesticides Results folder)7.4.2.15 Create data file name with current date (e.g. 14-8-

2017)7.4.2.16 Check (Auto-increment) box7.4.2.17 Set the Number of Unknown Sample (e.g.5)7.4.2.18 Set the tray (e.g. 1) & the vial # (e.g. 1) 7.4.2.19 Click (Next)

7.4.2.20 Check (Save Batch File) box, create batch file name with the same date as the file name in (C:\LabSolutions\Data\Project1\CMD\Pesticides Results\14-8-2017)

7.4.2.21 Click (Finish)7.4.2.22 A Batch Table will be created as below:7.4.2.23 Set the sample name &ID for the rest of the

samples

7.4.2.24 Set the dilution factor if present7.4.2.25 Set the sample amount if present7.4.2.26 Click (Start Realtime Batch) in the assistant bar

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7.5 Checking Analysis Results during Data Acquisition (Snapshot)7.5.1 You can take a snapshot to view the data during acquisition.

To take a snapshot7.5.2 Click (Snapshot) in the (Acquisition) assistant bar during

acquisition

7.6 Quantitative Data Analysis7.6.1 Open (LabSolutions Main) window7.6.2 Double-click (Postrun) to open (Data Analysis) window

7.6.3 The (Data Analysis) window can also be opened by clicking the (Data Analysis) icon in the (Acquisition) assistant bar

7.6.4 In the (Data Explorer) sub window, double-click to open the required Data file (e.g. 14-8-2017)

AFFsop 10, Rev 1 Page 10 of 13

7.6.5 Double-click on (Peak Integration for All IDs)

7.6.6 Maximize (Result View-Spectrum processing Table) sub window

7.6.7 Click on compound icon7.6.8 Check each compound for peak shape, retention time, ions

ratio and concentration

AFFsop 10, Rev 1 Page 11 of 13

7.6.9 Check (Calibration Curve) and the presence of all the transitions for each identified peak

7.6.10 Save the Data file7.6.11 Report the results according to (AFQP 521) in food test system

7.7 Shutdown7.7.1 Please note that the system should not be shutdown unless

required for scheduled maintenance7.7.2 Close any open (Data Analysis) window7.7.3 In (Realtime Analysis) window, click on (System control) icon

under (Main) assistant bar

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7.7.4 Click (Auto Shutdown)

7.7.5 Wait until finish then click (Close) 7.7.6 Exit LabSolutions7.7.7 Turn off the power to the LC modules7.7.8 Stop supplying all gases and plug DL with DL plug

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