scholarly journals Pesticide Residues Recovery studies by QuEChERS Sample Technique Using Gas Chromatography

2017 ◽  
Vol 104 (.1-.4) ◽  
Author(s):  
Sivanandha Reddy C ◽  
◽  
Subba Reddy G V
Keyword(s):  
Gas Chromatography ◽  
Sunflower Oil ◽  
Pesticide Residues ◽  
Preparation Method ◽  
Limit Of Detection ◽  
Sample Preparation Method ◽  
Limit Of Quantification ◽  
Target Analytes ◽  
Sample Technique ◽  
Standard Solution

The modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) sample preparation method was developed and validated for quantification of trace level of dicofol, chlordane and dieldrin pesticides in sunflower oil. The proposed method was applied for extraction of pesticides in sunflower oil and results were plotted with the help of matrix-matched calibration using relative responses versus standard solution. The quantification of pesticide residues carried out in sunflower oil by Gas Chromatography coupled with ECD detector. The method reveals that experimental results were satisfactory in respect of various analytical parameters such as linearity, recovery and precision. The limit of detection (LOD) and limit of quantification (LOQ) for target analytes were in the range of 0.001–0.011 mgkg-1 and 0.002–0.030 mgkg-1 respectively. The influence activated charcoal addition to the sorbents for the recovery of target analyte was also studied and presented in the results.

Determination of multiple organochlorine pesticide residues in shrimp using modified QuEChERS extraction and gas chromatography

2018 ◽  
Vol 16 (1) ◽  
pp. 81-93
Author(s):  
MDH Prodhan ◽  
SN Alam
Keyword(s):  
Gas Chromatography ◽  
Organochlorine Pesticide ◽  
Pesticide Residues ◽  
Limit Of Detection ◽  
Residue Analysis ◽  
Limit Of Quantification ◽  
Modified Quechers ◽  
Endosulfan Sulphate ◽  
Organochlorine Pesticide Residues

Determination of organochlorine pesticide residues in shrimp is very important to ensure the consumer’s safety and to fulfill the importer’s demand. Therefore, a simple and efficient multiple organochlorine pesticide residues analytical method using quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique and Gas Chromatography coupled with Electron Capture Detector (ECD) has been developed and validated for the determination of 19 organochlorine pesticides (α- BHC, δ- BHC, β- BHC, γ- BHC, Heptachlor, Aldrin, Heptachlor Epoxide, γ- Chlordane, α- Chlordane, α- Endosulfan, 4,4 DDE, Dieldrin, Endrin, 4,4 DDD, β- Endosulfan, 4,4 DDT, Endosulfan sulphate, Methoxychlor, and Endrin Ketone) in shrimp. The method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 84% to 106% with RSDr ≤ 14% in four fortification levels of 0.05, 0.1, 0.2 and 0.3 mg kg-1. The linearity was ≥ 0.996 for all of the selected pesticides with matrix matched calibration standards. The LOD ranged from 0.003 to 0.009 mg kg-1 and the LOQ was 0.05 mg kg-1. This method was applied successfully for the residue analysis of 40 shrimp samples collected from different regions in Bangladesh.SAARC J. Agri., 16(1): 81-93 (2018)

scholarly journals Development of a simple HPLC procedure for the determination of prochloraz residues in mushrooms

2021 ◽  
Author(s):  
Csaba Csutoras ◽  
Andras Misz ◽  
Csaba Nagy-Koteles ◽  
Nora Bakos-Barczi ◽  
Laszlo Racz
Keyword(s):  
Preparation Method ◽  
Limit Of Detection ◽  
Sample Preparation Method ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Mushroom Production ◽  
Modified Quechers ◽  
Cost Efficient ◽  
Solid Liquid

AbstractA simple HPLC-UV procedure is described in our paper which is suitable for the rapid and cost-efficient determination of prochloraz in mushrooms. Prochloraz is the only fungicide in EU which use is allowed in mushroom production. The aim of our work was the development of a simple method that is suitable for the control of this pesticide in everyday analyses during mushroom production. The procedure involves a simple sample preparation method based on solid-liquid extraction (modified QuEChERS extraction method EN 15662) followed by an HPLC-UV determination (recovery: 97–99%; limit of detection LOD: 0.01 mg/kg; limit of quantification LOQ: 0.05 mg/kg).

scholarly journals Development and method validation for determination of 54 pesticides in Okra by LC-MS/MS analysis

2020 ◽  
Vol 11 (1) ◽  
pp. 985-992
Author(s):  
Hymavati Muppalla ◽  
Kiranmayi Peddi
Keyword(s):  
European Union ◽  
Pesticide Residues ◽  
High Performance ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Mass Spectrometry Analysis ◽  
Limit Of Quantification ◽  
Spectrometry Analysis ◽  
Tandem Mass Spectrometry Analysis

The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers across the globe. The aim of the present study was to assess the level of pesticide residues in Okra in India. A multi-residue method for the quantification of fifty-four pesticides in okra is described in this work. The present study employed a modified quick, easy cheap, effective rugged and safe (QuEChERS) extraction procedure followed by UHPLC-MS/MS (Ultra-High-Performance Liquid Chromatography coupled to Tandem Mass Spectrometry) analysis. Validation of the method was according to the guidelines given by European Union SANCO/12571/2013. The levels of validation were 10.0, 50.0 and 100 µg kg-1. The following parameters such as linearity, the limit of detection (LOD) (nearer to 0.005 mg kg-1) and limit of quantification (LOQ) (nearer to 0.01 mg kg-1) were set to be acceptable. The trueness of the method for 54 pesticides in all Okra commodities was between 80-110% with satisfactory repeatability and within-run reproducibility except for the pesticide residues such as Thiamethoxam and Fenamidone. The measurement of uncertainty for each of the pesticide was below 50% and was estimated to be in the range of 5.37% - 10.71%, which meets the criteria established in the SANCO/12571/2013 document (European Union, 2013). This method is concluded to be applicable for the determination of pesticide residues in Okra.

scholarly journals VALIDATION AND ANALYSIS OF DIALLYL DISULFIDE AND DIALLYL TRISULFIDE IN GARLIC (ALLIUM SATIVUM L.) USING GAS CHROMATOGRAPHY

2020 ◽  
pp. 163-166
Author(s):  
HARMITA HARMITA ◽  
HERMAN SURYADI ◽  
LIDWINA DEVIANI LIKASA
Keyword(s):  
Gas Chromatography ◽  
Allium Sativum ◽  
Limit Of Detection ◽  
Diallyl Disulfide ◽  
Diallyl Trisulfide ◽  
Ionization Detector ◽  
Limit Of Quantification ◽  
Flame Ionization ◽  
Precision Limit ◽  
Optimized Conditions

Objective: The purpose of this research was to optimize and validate a method for measuring the levels of diallyl disulfide (DADS) and diallyl trisulfide(DATS) in garlic and single clove garlic.Methods: The analysis was performed using gas chromatography (GC) equipped with an HP-1 column and a flame ionization detector. The initialcolumn temperature was set at 140°C and increased at 1°C/min to 180°C. The injector and detector temperatures were set to 200°C, the carrier gasflow rate was 0.80 mL/min, and the injection volume was 1.0 μL. The optimized conditions of analysis were then validated which included selectivity,linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ).Results: Using the validated assay and a concentration range of 0.5–20 μg/mL, the coefficient of correlation (r) for DADS was 0.9999 and the LODand LOQ for DADS were 0.3063 μg/mL and 1.0210 μg/mL, respectively. Using the validated assay and a concentration range of 0.5–20 μg/mL, thecoefficient of correlation for DATS was 0.9999 and the LOD and LOQ for DATS were 0.1986 μg/mL and 0.6621 μg/mL, respectively. The percentage ofrecovery was in the range of 98.05–101.76% and coefficient of variation ≤ 2%.Conclusion: This GC method accurately measures the levels of DADS and DATS in garlic.

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