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KMID : 1023520110340040429
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Korean Journal of Veterinary Service
2011 Volume.34 No. 4 p.429 ~ p.439
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Comparison between the Liquid-Liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat
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Kim Yoen-Joo
Choi Yoon-Hwa
Shin Bang-Woo
Lee Jung-Hark
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Abstract
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This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of C18 and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3∼5.0 μg/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3∼6.2 μg/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).
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KEYWORD
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Pesticide residue, QuEChERS, GC-tandem mass spectrometry
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