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http://dx.doi.org/10.5338/KJEA.2018.37.4.42

Study for Residue Analysis of Herbicide, Clopyralid in Foods  

Kim, Ji-young (Division of Import Food Analysis, Ministry of Food and Drug Safety-Seoul Region, Ministry of Food and Drug Safety)
Choi, Yoon Ju (Food Standard Division, Food Standard Planning, Ministry of Food and Drug)
Kim, Jong Su (Division of Import Food Analysis, Ministry of Food and Drug Safety-Seoul Region, Ministry of Food and Drug Safety)
Kim, Do Hoon (Division of Import Food Analysis, Ministry of Food and Drug Safety-Seoul Region, Ministry of Food and Drug Safety)
Do, Jung Ah (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Jung, Yong Hyun (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Lee, Kang Bong (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Kim, Hyo Chin (Division of Import Food Analysis, Ministry of Food and Drug Safety-Seoul Region, Ministry of Food and Drug Safety)
Publication Information
Korean Journal of Environmental Agriculture / v.37, no.4, 2018 , pp. 283-290 More about this Journal
Abstract
BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.
Keywords
Clopyralid; LC-MS/MS; Residue;
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