Analysis of pesticide residues in drinking water samples using solid-phase micro-extraction (SPME) coupled to a gas chromatography-electron-capture detector (GC-ECD)

2011 ◽  
Vol 11 (6) ◽  
pp. 754-764 ◽  
Author(s):  
Prashant Chaturvedi ◽  
Rupender Kumari ◽  
Ramesh Chandra Murthy ◽  
Devendra Kumar Patel

The headspace solid-phase micro-extraction (HS-SPME) method with polydimethylsiloxane (PDMS, 100 μm) fiber is a cost-effective technique for the determination of different pesticide residues in environmental and biological samples followed by a gas chromatography-electron-capture detector (GC-ECD). In the present study more than 147 water samples collected in and around Lucknow city were analyzed. The method detection limits and recovery percentages were found in the ranges of 0.05–0.20 μg/L and 87.1–95.3% respectively. The average concentration of organochlorine and organophosphorus pesticides in water samples within the city were ranged between 0.258–0.829 μg/L and 0.143–0.294 μg/L respectively. Organochlorine and organophosphorus pesticides in highway water samples ranged between 0.261–2.80 μg/L and 0.129–0.53 μg/L. Pyrethroid pesticides were not found in any of the water samples tested. The levels of pesticide residues were compared with their MRL values recommended by the Prevention of Food Adulteration Act (PFA), Government of India (1954).

Author(s):  
Devendra Kumar Patel

A fast, simple, solvent less and inexpensive sample preparation method based on Head space solid-phase micro extraction (HS-SPME) coupled to gas chromatography-electron-capture detector (GC-ECD) is proposed for the determination of mix pesticide residues from vegetable samples. Polydimethylsiloxane (PDMS, 100 μm) fiber was used in this study. The mix pesticides (24 nos.) including organochlorines (15), organophosphates (06) and synthetic pyrethriods (03) were analysed in the vegetable samples (Cabbage, Tomato, Cauliflower, Chilli, Okra, Brinjal, Bottle gourd, Cucumber, Beetroot, Spinach, and Radish) collected from in and around of Lucknow city, India. Present study revealed the presence of HCH, DDT, methylparathion, malathion, chlorpyrifos, monocrotophos, endosulfan, cypermethrin, fenvalerate pesticides. Pesticides residue levels were compared with MRL fixed by Prevention of Food Adulteration Act (PFA), Govt. of India 1954. The method detection limits were in a linearity range of 0.003 - 0.024 mg/kg. A recovery percent varies from 86.1 to 96.4% with relative standard deviation (RSD) of 14%. The outcomes of the present study point towards the crucial need of implementing strict government’s rules related to food safety in order to put check on these kinds of health hazardous food contamination.


2006 ◽  
Vol 89 (5) ◽  
pp. 1437-1442 ◽  
Author(s):  
Suxia Zhang ◽  
Fengyun Sun ◽  
Jiancheng Li ◽  
Linli Cheng ◽  
Jianzhong Shen

Abstract A rapid and sensitive gas chromatography method was developed for the simultaneous determination of florfenicol (FF) and its metabolite florfenicol amine (FFA) in fish, shrimp, and swine muscle. The extracted samples were defatted with hexane and cleaned up by solid-phase extraction using Oasis MCX cartridges. The eluate was evaporated to dryness, and residues were derivatized and determined by gas chromatography with a microcell electron capture detector. Overall average recoveries ranged from 81.7 to 109.7% for fish, 94.1 to 103.4% for shrimp, and 71.5 to 91.4% for swine muscle. The detection limit was 0.5 ng/g for FF and 1 ng/g for FFA, respectively. The method was validated for the determination of incurred swine muscle samples in an actual residue study.


1996 ◽  
Vol 79 (6) ◽  
pp. 1423-1427 ◽  
Author(s):  
Rosario Garcia-Repetto ◽  
Isabel Garrtoo ◽  
Manuel Repetto

Abstract A multiresidue analytical method is described for determining 6 pesticides in wine: chlorpyrifos, dimethoate, quinalphos, simazine, tetradifon, and endosulfan. Wine (200 mL) is extracted with dichloromethane (50 mL, 3 times), and the evaporated extracts are purified by silica gel chromatography. Pesticide residues are eluted with n-hexane, n-hexane-benzene (1 + 1), benzene, benzene–acetone (1 + 1), and acetone. Residues are determined by gas chromatography with nitrogen–phosphorus and electron capture detection, using CPSH-5CB, Carbo wax-20M, and CPSH-19CB columns. Recoveries of pesticides added at 0.025 μg/L were 83–97%, with standard deviations of 0.01–0.05%. Detection limits were 0.13–8.9 ng/L, except for simazine (36.7 μg/L). Results are compared with those obtained with a solid-phase extraction (C18) purification and with different eluant series.


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