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Assignment ACCE 514

This document describes a study analyzing organophosphate pesticides in food samples using gas chromatography. The study developed a method to detect chlorpyrifos-methyl, triadimefon, penconazole, hexaconazole, and diniconazole in eggplant and tomato samples. Samples were extracted with acetonitrile then analyzed using gas chromatography with electron capture, nitrogen phosphorus, and flame ionization detectors. The method achieved good separation of analytes in 17 minutes and was successfully applied to real food samples.

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Naimmul Fahim
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35 views4 pages

Assignment ACCE 514

This document describes a study analyzing organophosphate pesticides in food samples using gas chromatography. The study developed a method to detect chlorpyrifos-methyl, triadimefon, penconazole, hexaconazole, and diniconazole in eggplant and tomato samples. Samples were extracted with acetonitrile then analyzed using gas chromatography with electron capture, nitrogen phosphorus, and flame ionization detectors. The method achieved good separation of analytes in 17 minutes and was successfully applied to real food samples.

Uploaded by

Naimmul Fahim
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Bangabandhu Sheikh Mujibur Rahman Science

and Technology University, Gopalganj-8100

An assignment on
Detection of Organophosphate in Food Sample by Gas
Chromatography
Course Code: ACCE 514
Course Title: Food Processing Engineering

Submitted to
Rifat Ara Masud
Lecturer
Dept. of Applied Chemistry and Chemical Engineering, BSMRSTU

Submitted by
Md. Nahidul Islam Sajol
Id. no. 20151107021
Master’s 1st Semester
Dept. of Applied Chemistry and Chemical Engineering, BSMRSTU

Date of Submission: 25.11.2020


Gas chromatography with selective detectors is the analytical method generally used for
determining pesticide residues in food sample. Organophosphorus compounds are reliably
detected with a phosphorus-specific flame photometric detector (FPD), electron-capture
detection (ECD), nitrogen-phosphorus detection (NPD), or flame ionization detection (FID)
has been developed for the determination of organophosphorus residues such as chlorpyrifos-
methyl. The method has been successfully applied to the analysis of tomatoes and eggplant
food samples. A major problem arises from the great number of compounds to be analyzed
which has increased to the point where it is almost impossible to separate them all in a single
chromatogram. This applies even to high performance capillary columns. Measurement of
retention time on one single column is definitely not sufficient for the identification of a
pesticide. It therefore becomes necessary to re-run the sample on one or two columns of
different polarity.1

Procedure

Chemicals
Chlorpyrifos-methyl, triadimefon, penconazole, hexaconazole, and diniconazole certified
standards is collected. Stock solutions (0.1mgmL-1) is prepared, by dissolving the selected
organophosphate compounds such as chlorpyrifos-methyl in acetone and stored in the dark at
4℃. More diluted solutions within the concentration range 1.0–10 mgmL-1 prepared from
stock solution just before use. Sodium chloride 99.5% is used. Anhydrous sodium sulfate was
pesticide residue analysis. Other chemicals such as acetonitrile and acetone are analytical
grade reagents.2

Apparatus
An Agilent 6890N Gas chromatography equipped with an split/splitless capillary injection
port, a nitrogen phosphorus detector (NPD), and electron capture detector (ECD) with
capillaries HP-1MS Agilent 19091S-933 (100% dimethyl siloxane, 30m× 0.25mm i.d., 0.25
mm film thickness) and HP-5MS Agilent 19091 J-433 (5% phenylmethyl siloxane, 30m ×
0.25mm i.d., 0.25 mm film thickness) are used, respectively. Agilent 6890N gas
chromatography equipped with an flame ionization detector (FID) with capillaries HP-5
Agilent 19091 J-433 (5% phenylmethyl siloxane, 30m ×0.32mm i.d., 0.25 mm film
thickness) is also used.2

The oven temperature program is 80°C for 2 min, increased from 80 to 220°C at 80°C/min,
held at 220°C for 0.0 min; increased to 260°C at 3°C min-1, held at 260°C for 0.0 min. The
carrier gas (helium) flow rate is in constant flow mode at 1.0mL min-1. Splitless injection of
1 mL volume is carried out at 250°C. Temperature for the detectors was 300°C. Supporter
gas for ECD was nitrogen with a flow rate of 60mL min-1. Detector gas for NPD was
hydrogen and dry air with a flow rate 3.0mL min-1 and 60.0mL min-1, respectively and
helium was supporter gas (10mLmin-1). For FID, hydrogen, and dry air are used with a flow
rate 3.0mL min-1 and 60.0mL min-1, respectively. The supporter gas was helium with a flow
rate of 25mL min-1. The total analysis time was 17.08 min and finally for calculations.2
Sample Preparation
Samples are collected from a pesticide free area where organic agriculture has being done.
Eggplant and tomatoes samples are prepared for analysis. A 10 g sample of food is
homogenized in a food processor and placed in a polypropylene centrifuge tube. Aliquot of
previously homogenized sample of eggplant and tomatoes are spiked with 0.5mL of working
solutions (10 mgmL-1 of chlorpyrifos-methyl, triadimefon, penconazole, hexaconazole,
diniconazole mixture) and mixed by vortexing for one min. The samples are extracted with
9.5mL of acetonitrile in a homogenizer. Then, 4.0 g of anhydrous magnesium sulfate and 0.5
g of sodium chloride are added and the resulting mixture centrifuged at 6000 rpm for 5 min.
The 2.0mL of extract is transferred into the 15mL centrifuge tube containing 300mg
anhydrous MgSO4, 50mg primary secondary amine (PSA), and 50mg chromabond diamino.
It is vortexed for 2 min and centrifuged at 6000 rpm for 5 min. Acetonitrile is evaporated
from 1.0mL extract under the nitrogen atmosphere and dissolved in 1mL of acetone before
injection.2

Discussion
In this analysis, some organophosphate pesticides namely such as chlorpyrifos-methyl,
triadimefon, penconazole, hexaconazole, and diniconazole, three detectors (ECD, NPD, and
FID) and three different columns (HP-5S, HP-1MS, and HP-5) are investigated under the
same optimized temperature programs and analysis time, to obtain the most efficient
quantitative results with maximum separation. Each pesticide is injected and retention times
are recorded. In the case of close retention times, separation by changing temperature
programs is achieved. Several tests are performed in order to obtain the best optimized
separation-resolution of the analytes used. The GC operating conditions and optimized oven
temperature programs are explained in Experimental section. The chromatograms of the
standard organophosphates compounds for their multiple analyses are successfully obtained
under optimized conditions. The applied temperature program resulted in a good separation
of the analytes by employing the stated chromatographic conditions. The mixture of five
compounds under study was well resolved in a run time of 17.08 min.2

References

1. Stan H ‐J, owetz D. Residue analysis of organophosphorus pesticides in food with two‐
dimensional gas chromatography using capillary columns and flame photometric
detection. J High Resolut Chromatogr. 1983;6(5):255-263.
doi:10.1002/jhrc.1240060507

2. Güdücü HE, Inam R, Aboul-Enein HY. Determination of organophosphorus and


triazole pesticides by gas chromatography and application to vegetable and
commercial samples. J Liq Chromatogr Relat Technol. 2011;34(19):2473-2483.
doi:10.1080/10826076.2011.591027

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