RESIDUAL PESTICIDES ANALYSIS OF VERIOUS ...3.Department of Earth & Environmental Science, KSKV...

Bhatt et al RJLBPCS 2019 www.rjlbpcs.com Life Science Informatics Publications

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2019 Jan – Feb RJLBPCS 5(1) Page No.53

Original Research Article DOI: 10.26479/2019.0501.06

RESIDUAL PESTICIDES ANALYSIS OF VERIOUS VEGETABLES BY GC-MS

Jyotindrakumar J Bhatt1*, H. P. Gajera2, Daya B. Dobariya1, Mrugesh H Trivedi3

1.Department of Chemistry, KSKV Kachchh University, Bhuj, Gujarat, India.

2.Department of Biotechnology, Junagadh Agriculture University, Junagadh, Gujarat, India.

3.Department of Earth & Environmental Science, KSKV Kachchh University, Bhuj, Gujarat, India

ABSTRACT: This reported work describes residual pesticide analysis in different vegetables, during the

period first quarter of the year. A Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method

(AOAC Official Method 2007.01) was used to extract pesticide residues from vegetable samples. The

vegetable, fruits and grain market-yard of Junagadh the district place of Gujarat is the selected place from

which the vegetables are collected. In this study we reported the determination of pesticide residues from

selected eight vegetables like cauliflower, brinjal, tomato, cabbage, cluster bean, bottle guard, okra, and chili.

The samples were prepared by usual and established method and followed by extraction were subjected to

analyses. The extracted pesticide residues were analyzed and quantified by standardized Gas

Chromatography/Mass Spectrometry (GC-MS) method developed for 35 pesticide standards. The literature

survey of the study of various samples, we tempted to do further study for the residue pesticides and residual

insecticides analysis with more interest of its penetration and quantification in vegetables in order to

understand the adverse effects and toxicity. The results indicate the presence of pesticide residues in some of

the samples above the stated MRL (Maximum Residue Limit) value.

KEYWORDS: Pesticides, GC-MS, Vegetables, Human Health.

Corresponding Author: Dr. Jyotindrakumar J Bhatt*Ph.D.

Department of Chemistry, KSKV Kachchh University, Bhuj, Gujarat, India.

Email Address: [email protected]

1.INTRODUCTION

The aim of this undertaken work is to describe the pesticide residue in fruit and vegetable, mainly

how they are introduce, dissipated and degraded. Vegetable are important components of human diet

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since they provide essential nutrients that are required for most of the reactions occurring in the

body. A high intake of fruits and vegetables has been encouraged not only to prevent consequences

due to vitamin deficiency but also to reduce the incidence of major diseases such as cancer,

cardiovascular diseases and obesity. Like other crops, vegetables are attacked by pests and diseases

during production and storage leading to damages that residue and quality and the yield. [1, 2]. A

pesticide can also be introduce according to their, Chemical substance, application on different

Biological agents (such as virus or bacteria), as disinfectant, antimicrobial agent or its using like

device. The Pesticide residue refers to the pesticides that may remain on or in food after they are

applied to food crops. The levels of these residues in foods are often stipulated by regulatory bodies

in many countries. Exposure of the general population to these residues most commonly occurs

through consumption of treated food sources, or being in close contact to areas treated with

pesticides such as farms or lawns around houses [3].Pesticides are often referred to according to the

type of pest they control. Another way to think about pesticides is to consider those that are chemical

pesticides or are derived from a common source or production method. Other categories include bio

pesticides, antimicrobials, and pest control devices. Once it reaches the target pest, the chemical

may act in different way likewise,blocking the cellular processes of target organisms in a purely

mechanical way, by this the pesticide physically prevents a basic cellular function even without any

chemical reactions. Destroy or alter the pest’s metabolism. Examples include inorganic copper

compounds, dithiocarbamate fungicides, phosphono amino acid herbicides and organophosphate

insecticides [4].The application of pesticides has a significant effect on biodiversity. These affect

the ability of soil to regenerate itself and remain viable for plant and animal life [5].Environment

devastated by pesticides may take years to recover. In some cases, it may never recover at

all!Maximum residue levels are the highest levels of residues expected to be in the food when the

pesticide is used according to authorised agricultural practices. The MRLs are always set far below

levels considered to be safe for humans. Safety limits are assessed in comparison with acceptable

daily intake (ADI) for short term exposure or acute reference dose (ARfD). MRLs are subject to

legal requirements in most of the countries. MRL setting is based on the national registered good

agriculture practice (GAP) data combined with the estimated likely residue from the supervised

trials mean residue (STMR), ADI and ARfD. MRLs may be exceeded because of pesticide misuse,

false positives due to naturally occurring substances, differences in national MRLs, lack of

registered pesticides and incorrect pesticide application [6]. In this present study, systematic path

way for residual pesticide analysis have been developed. Generally pesticides occur in food in very

low concentration, usually at ppm level. Measuring such a small amount of pesticides is the function

of pesticide residue analysis. A variety of analytical methods are currently used to detect pesticide

residue, and contain certain basic steps, that include, Sampling (Sampling procedure for






vegetablesby collection, transport and storage of sample) [7]. Detection is based on Trace Level

Analysis of Pesticide Residues [8]. Extraction method for pesticide residue analysis [9]is having

special attention of the researchers.The residues of pesticides have been generally analyzed by gas

chromatography with different detectors. High performance liquid chromatography (HPLC) [10]

has been also employed, particularly when pesticides are thermally instable. Gas chromatography

coupled with mass spectrometry (GC-MS) is more often used at present for pesticide analysis from

soil [11-17] due to the possibility of confirming pesticide identity. The main objective of this work

was to develop a rapid and simple multi residue method for the analysis of pesticides in our samples,

based on the QuEChERS extraction method using a low volume of organic solvent and their

determination by GC-MS[18].

2. MATERIALS AND METHODS

The present experimental work on collecting samples and extractions have been carried out

systemically in order to approach the system which established from reported survey [19-30].

Analyses was done by the Equipments utilized for sample preparation are like, Centrifuge :REMI

Research centrifuge, Vortexer : GeNeiTm, Turbovapour: Caliper Turbovap L-6,Analytical

Balance:0.1 mg – 5.0 gm (LC-GC Analyticals), Auto-Pipette: volume range Genaxy(GENPET Auto

Pipette), 0.2Micron nylon membrane filters from Himedia and finally GCMS System: GC-2010 plus

(Shimadzu).

Sample preparation for QuEChERS

Organic bottle top dispense, Trace HP-5MS Pesticide (length 30m,diameter 0.250mm, fit thickness

0.25 µm),2 mL amber glass vile, 50 ml FEP centrifuge tubes, Clean up tube: 15 mL tubes , Clean

up tube: 2 mL tubes have been taken for preparation and preservation of our samples. Reagents and

chemicals that used for treating samples are 15 ml of 1% acetic acid, Acetonitrile (v/v) HPLC

grade,6 gm MgSO4 (anhydrous) and 1.5 gm sodium acetate(anhydrous),ENVIRO 900 mg MgSO4,

300 mg PSA 150 mg, 150 mg MgSO4, 50 mg PSA (pk of 100). The Standard pesticide stock

solutions were prepared by diluting 1.00mg of each standard pesticide in 10.00mL of HPLC grade

(Fisher scientific) ethy-l acetate. The final concentration was 1.00 mg/mL or 100 ppm. For each

pesticide standard mentioned above, Stock Solutions (SS) of 100 ppm concentration were prepared

in ethyl acetate. A pesticide intermediate standard solution Stock Dilution (SD) 10ppm was prepared

by transferring 1 mL from each pesticide Stock Solutions (SS) to a 15ml tarsons tube and diluting

to volume with ethyl acetate to obtain a concentration of 100µg/mL.The stock dilutions were then

further diluted to prepare Working Solutions (WS) of 1 ppm concentration in ethyl acetate. The

working solutions were then used to prepare pesticide standard solution of 500 ppb, 200 ppb, 100

ppb, and 50 ppb and 10 ppb concentrations. The pesticide standard solutions of 10 ppm was used to

tune the instrument for pesticide residue analysis in the scan mode, while pesticide standard






solutions of 1ppm, 500 ppb, 100 ppb, 50 ppb and 10 ppb concentrations were used to tune the

instrument in the SIM (Selective Ion Monitoring) mode.

Instrument: GC-MS - Model:- QP2010 Plus Table 1: Criteria, parameter with condition

Table 2:Method development of Pesticide Standards for Pesticide Residue Analysis

GC-Program

Column: HP-5MS (Crossbond, 5% diphenyl / 95% dimethylpolysiloxane)

30 m x 0.25 mm I. D. df = 0.5 µm

Column Oven

Temperature Program:

- Initial temp.120 oC hold for 1 min;

- Temp. ramping 8 oC /min, upto 150

oC, hold for 1 min;


oC, hold for 1 min;


oC, hold for 2 min;


oC, hold for 2.5 min.

Carrier Gas: Helium (99.999% pure)

Injection Temperature: 280 ºC

Injection Method: Splitless (1 min), high pressure injection @ 250 psi

Injection Volume: 1 µL

Total Run Time: 42.50

Solvent cut time: 4.0 min

Interface Temperature: 290 ºC

Ion source Temperature: 230 ºC

Ionization Mode: EI (Electron Ionization)

Scan Range: 50-500 m/z

Pesticide Standard

Mobile Phase

Retention Time

(min)

Ionization

Mode (A) 0.1 % Formic Acid

in MilliQ (B) Acetonitrile

Imidacloprid 90% 10% 0.34 ESI +

Thiamethoxam (50%) (50%) 0.33 ESI +

Thiodicarb (90%) (10%) 0.33 ESI +

CartapHydrochloride (90%) (10%) 0.34 ESI +

Diafenthiuron (10%) (90%) 0.55 ESI +

Imazethepyr (90%) (10%) 0.49 ESI +






LC-MS-MS method: Model: Waters Acquity UPLC-PDA, TQD mass detector. Extraction

Method& Quantification of Pesticide Residues from vegetables:

Vegetables Sampling:Vegetable sampling was done from the Junagadh District of Gujarat. 8

different type of vegetables namely, Cabbage (V1), Cauliflower (V2), Cluster Bean (V3), Bottle

guard (V4), Okra (V5), Brinjal (V6), Chilli (V7), and Tomato (V8) were collected from the Junagadh

Vegetable Marketing Yard.

Procedure for sampling:

1 Kg of each vegetable was purchased from two different vendors. They were then mixed and stored in

polyethylene bags and labeled properly. They were stored in the laboratory at 2°- 8°C until analyzed.

V1- Cabbage V2-Cauliflower V3-Clusterbean

V4 - Bottle gourd V5- Okra V6- Brinjal

V7– Chilli V8– Tomato






QuEChERS sample preparation

The determination of pesticides in fruits and vegetables has been simplified by a new sample

preparation method, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), and published

recently as AOAC Method 2007.011 The sample preparation is shortened by using a single step

buffered acetonitrile (MeCN) extraction and liquid-liquid partitioning from water in the sample by

salting out with sodium acetate and magnesium sulphate (MgSO4). The MeCN extract is solvent

exchanged to hexane/acetone for split less injection with detection by electron ionization and

selected ion monitoring (SIM).

Experimental condition

During the method validation, several experiments were performed to determine the effect of minor

modification to the QuEChERS method which may impact the performance of the analysis in the

laboratory. The recommended consumables required for sample preparation and analysis were

austerely tested (Table 3). The sections were evaluated for sample preparation are,Sample Extraction

and Clean Up, Solvent Exchange, Injection, Separation, Detection

3. RESULTS AND DISCUSSION

Different vegetables viz. Cabbage (V1), Cauliflower (V2), Cluster Bean (V3), Bottle guard (V4),

Okra (V5), Brinjal (V6), Chilli (V7), and Tomato (V8) were collected from market yard of Junagadh

(Gujarat) and studied. The residue concentrations were calculated using reference standards. Out of

35pesticides, total 18 pesticide residues like Trifluralin, Cypermethrin, Propiconazole, Quizalofop-

Ethyl, Pendimethalin, Triazophos, Fenpropathrin, Propiconazole, Carbofuran,alpha-Lindane, beta-

Lindane, gamma-Lindane, Endosulfan-2, delta-Lindane, Methyl-Parathion, Alachlor, Butachlor and

Ethion were detected among 8 vegetables. The maximum residues (Nine pesticides) were detected

in Okra followed by Brinjal (Six pesticides). However, least residue (One-Propiconazol) was Bottle

guard. In cabbage, three residues were detected among which the concentration of Triazophos was

found higher. Cauliflower has two pesticide residues with Quizalofop-Ethyl as higher, while

Pendimethalin was detected higher in cluster bean. Okra has five pesticide residues among which

two pesticides Lindane and Cypermethrin have their isomers (three for each). Thus, total nine

residues including their isomers were detected in Okra. Brinjal has 6 residues with Carbofuran as

highest one, while Chilli sample had four pesticide residues among which Butachlor was found

higher. Methyl-Parathion was detected higher in tomato in addition to two other pesticide residues.

Among all the pesticide residues detected in all the vegetable samples, the concentration of

Butachlor was highest, while that of Endosulfan-2 was lowest, whose structures are as below.






Butachlor Endosulfan-2

Table 3:Pesticide residues quantified from samples

Name of

the vegetable &

Code No.

Pesticide(s) found Concentration

(mg/Kg)

MRLs (mg/ kg)

/ (As per std. of 2013)

Codex EU

V1

Cabbage

Trifluralin 0.027 - 0.01

Triazophos 0.156 - 0.01

Cypermethrin 0.056 1 1

V2

Cauliflower

Propiconazole 0.076 - 0.05

Quizalofop Ethyl 0.088 - 0.04

V3

Cluster bean

Pendimethalin 0.598 - 0.05


Fenpropathrin 0.401 - 0.01

V4

Bottle gourd

Propiconazole 2.602 - 0.05

V5

Okra

Carbofuran 0.021 - 0.01

alpha-Lindane 4.304 - 0.01

beta-Lindane 0.133 - 0.01

gamma-Lindane 0.400 - 0.01

Endosulfan-2 0.021 0.5 0.05


Cypermethrin-1 0.196 0.1 0.05



V6

Brinjal

Carbofuran 1.789 - 0.01

Trifluralin 0.046 - 0.01

gamma-Lindane 0.475 - 0.01

delta-Lindane 0.442 - 0.01

Methyl-Parathion 0.102 - 0.01


V7 beta-Lindane 2.126 - 0.01






Figure 1: Chrometograph-1

Figure 2: Chrometograph-2

Chilli Alachlor 0.299 - 0.01

Butachlor 13.006 - -

Ethion 0.161 - 0.01

V8

Tomato

Methyl Parathion 0.610 - 0.01

Alachlor 0.072 - 0.01


5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5 35.0 37.5

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

1.1

1.2

1.3

1.4

1.5

1.6(x10,000,000)

TIC

12

3 45

67

89

10

11

12

131

41

5

16

17

18

19

20

21

22

23

24

25

26

27

28

29

30

31

32

33

34

35

36

37

38

39

40

41

42

43

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5 35.0 37.5

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

1.1

1.2

1.3

1.4

1.5

1.6(x10,000,000)

TIC

12

3 45

67

89

10

11

12

131

41

5

16

17

18

19

20

21

22

23

24

25

26

27

28

29

30

31

32

33

34

35

36

37

38

39

40

41

42

43






Development of Calibration Curve of Pesticide Standards

1 μL of mixture of 35 pesticide standards at different working concentration (500 ppb, 100

ppb 50 ppb and10 ppb) were injected in to the developed and SCAN mode and SIM.

Table 4:Straight Line Equation and R2

Value of each pesticide standard in CC Set

Sr.No. Pesticide Standard Straight Line Equation R2 value

1. Carbofuran Y = 9616.542X + 25394.2 0.9985434

2. Trifluralin Y = 2373.789X +9891.049 0.9977985

3. Phorate Y = 7168.044X +27948.38 0.9992948

4. Dimethoate Y = 1967.341X -27528.05 0.9961004

5. Fluchloralin Y = 1840.894X + 3704.859 0.9989157

6. Methyl-Parathion Y = 1826.126X +12287.39 0.9859142

7. Alachlor Y = 3772.375X -28848.37 0.9990137

8. Heptachlor Y = 1929.796X -9616.518 0.9979476

9. Malathion Y = 2102.9X - 75749.91 0.9983016

10. Chlorpyriphos Y = 4353.934X+90131.99 0.9963005

11. Aldrin Y = 3374.273X+15733.85 0.998087

12. Pendimethalin Y = 1299.304X -2768.327 0.9979654

13. Butachlor Y = 5011.607X +26036.97 0.9843095

14. Endosulfan-1 Y = 574.0606X + 16593.61 0.9990655

15. Profenofos Y = 643.1272X -9073.941 0.9741099

16. Endosulfan-2 Y = 1194.472X +15636.13 0.9965006

17. Ethion Y = 3930.323X -68253.03 0.9933582

18. Triazophos Y = 1930.781X -53887.57 0.982844

19. Quizalofop-ethyl Y = 3870.936X -145147.5 0.9901825

20. Cabaril Y = 9616.542X +25394.2 0.9985434

21. a-BHC Y = 94.4106X +94108.07 0.6315221

22. b-BHC Y = 1212.904X +6387.056 0.9995311

23. g-BHC Y = 769.121X + 29049.18 0.9642116

24. d-BHC Y = 756.0549X +57914.01 0.9918748

25. Fluchlolalin Y = 1840.894X +3704.859 0.9989157

26. Fipornil Y = 6936.443X -221473.4 0.9911576

27. Oxyflurofen Y = 831.2414X -29468.57 0.9895674

28. Propiconazol-1 Y = 1832.952X -32373.87 0.9992266






29. Propiconazol-2 Y = 2621.924X -41706.33 0.9990739

30. Bifenthrin Y = 9984.335X -82663.65 0.9991796

31. Fenpropethin Y = 7948.786X -90511.99 0.9993834

32. Cypermethrin Y = 2453.772X +126229.7 0.9720539

33. Fenvelarate Y = 2061.077X +156991.1 0.9785813

Figure: 3. Chromatogram of different vegetables sample

(black-V1, pink—V2, blue-V3, brown-V4, green-V5, purpal-V6, light green-V7, black-V8)

DISCUSSION

1µL of mixture of 35 pesticide standards at different working concentration (1 ppm, 500 ppb, 100

ppb and 50 ppb) were injected in to the developed and optimized GC-MS method. Depending on

the retention time obtained from analysis of each individual pesticide standard and relative reference

ions using Total Ion Chromatogram (TIC), the standard analyte in mixture were eluted and confirm

by similarity search from the inbuilt Pesticide Library an NIST Library.The peaks of each individual

pesticide standard obtained were integrated manually for each working concentration. A calibration

plot was developed depending upon Area vs. Concentration. From each individual CC plot of

standard, a straight line equation was obtain. From the straight line equation the concentration of

residues obtained from the vegetable sample will be quantified in ppb concentration.The

chromatogram of the mixture of 35 pesticide standards injected in a single run of GC-MS and the

retention time (RT) of each individual pesticide standards and their relative isomers, majored. There

was no effect of mixture of pesticide on retention time obtained when individual standards were






eluted. The peaks obtained show more than 80 % similarity with the inbuilt NIST and Pesticide

Library.Figure-shows the relative intensities of chromatogram obtained at different concentration of

pesticide mixture.Figure-shows the calibration plot of pesticide standards Phorate, Dimethoate,β-

BHC etc. As these pesticides residue were extracted from the collected vegetable samples used in

this study

Table 5: Retention Time, peak area and identified compounds from samples

VEGETABLE SAMPLE-V1 to V8

Sr. No.

Retentio

n Time

(min.)

Area

Straight Line

Equation from CC

Set

Concentration

of pesticide

Residues(ppb)

Compound

Identified

(Cabbage)

V1

11.65 60676 Y = 1212.904X

+6387.056 678.879 beta-Lindane

15.92 14777 Y = 3772.375X -

28848.37 758.016 Alachlor

21.08 28205 Y = 5011.607X

+26036.97 876.340 Butachlor

24.21 124481 Y = 3930.323X -

68253.03 268.752 Ethion

Cauliflower

V2

25.75 121835 Y = 1832.952X -

32373.87 237.637 Propiconazole

35.51 90473 Y = 3870.936X -

145147.5 356.645

Quizalofop

Ethyl

Cluster

Bean

V3

19.19 54303 Y = 1299.304X -

2768.327 600.314 Pendimethalin

24.81 57321 Y = 1930.781X -

53887.57 156.656 Triazophos

28.50 131939 Y = 7948.786X -

90511.99

640.204 Fenpropathrin

Bottle Guard

V4

25.75 121835 Y = 1832.952X -

32373.87

237.637 Propiconazole

Okara

V5

4.34 315855 Y = 9616.542X +

25394.2 875.456 Carbofuran

8.32 138767 Y = 94.4106X

+94108.07 875.980 alpha-Lindane






11.65 60676 Y = 1212.904X

+6387.056 678.879 beta-Lindane

12.76 44141 Y = 769.121X +

29049.18 245.968

gamma-

Lindane

23.32 126868 Y = 1194.472X

+15636.13 875.765 Endosulfan-2

24.81 57321 Y = 1930.781X -

53887.57 276.572 Triazophos

35.14 54641 Y = 2453.772X

+126229.7 2077.472

Cypermethrin

-1

35.45 72570 Y = 2453.772X

+126229.7 25.850

Cypermethrin

-2

35.65 100668 Y = 2453.772X

+126229.7 25.850

Cypermethrin

-3

Brinjal

V6

27.99 273240 Y = 9616.542X +

25394.2 875.456 Carbofuran

11.25 110074 Y = 1930.781X -

53887.57 156.656 Trifluralin

11.65 60676 Y = 1212.904X

+6387.056 245.968

gamma-

Lindane

12.96 88539 Y = 1212.904X

+6387.056 245.968 delta-Lindane

15.59 155723 Y = 1826.126X

+12287.39 355.469

Methyl-

Parathion

28.50 131939 Y = 7948.786X -

90511.99 640.204 Fenpropathrin

Chilli

V7

11.65 60567 Y = 1212.897X

+6387.056 678.669

beta-HCH

15.92 14767 Y = 3772.367X –

28848.37 758.011 Alachlor

21.08 27901 Y = 5011.589X

+26036.97 142.507 Butachlor

24.21 124468 Y = 3930.318X -

68253.03 268.752 Ethion






Tomato

V8

15.59 155723 Y = 1826.126X

+12287.39 355.469

Methyl

Parathion

15.92 14777 Y = 3772.375X -

28848.37 758.016 Alachlor

28.50 131939 Y = 7948.786X -

90511.99 640.204 Fenpropathrin

4. CONCLUSION

The results from the above study highlighted the presence of pesticide residues in samples. Some

different types of pesticides are present in one type of vegetable indicating the increasing amount of

use of pesticides. Hence, it can be absorb in vegetable samples in law to moderate amount. Study

has been done with systematic process via collection, preservation followed by extraction. The

standard method was applied to treat the collected vegetables for sample preparation. The standards

were taken as reference and each of for calibration in order to quantify and compare with known

molecules of pesticides. Identification of such type of pesticides has been done with compare to that

of known. The main objective was to conduct trace level analysis of pesticide residues from

vegetable samples using GC–MS technique. The well established QuEChERS method is used with

its physico-chemical parameters for extraction of pesticide residue. The extracts were reconstituted

in appropriate solvent such as ethyl-acetate and analyzed by GC–MS. Finally the analyzed samples

were quantified using calibration curve of 35 pesticide standards by GC–MS. The entire study is

fulfilling the aim to show the non-negligible presence of the pesticides in vegetable samples. Results

are indicating the adverse effects and toxicity of these pesticides also harmfulness for human being.

ACKNOWLEDGEMENT

Authors are thankful to the authorities of Gujarat Agricultural University, Junagadh and the

Department of Chemistry, KSKV Kachchh University, Bhuj for providing research facility.

CONFLICT OF INTEREST

Authors have no any conflict of interest.

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