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KMID : 0881720190340020140
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Journal of Food Hygiene and Safety
2019 Volume.34 No. 2 p.140 ~ p.147
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Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS
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Cho Sung-Min
Do Jung-Ah
Lee Han-Sol
Park Ji-Su
Shin Hye-Sun
Jang Dong-Eun
Choi Young-Nae
Jung Yong-Hyun
Lee Kang-Bong
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Abstract
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An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with MgSO4 (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using MgSO4, PSA (primary secondary amine), C18 (octade- cyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in posi- tive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels (0.001-0.25 μg/mL) and the coefficient of determination (R2) was above 0.99. Recovery results at three con- centrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard devia- tions) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.
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KEYWORD
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Pesticide, Quinoxyfen, Fungicide, Analytical method, Agricultural product, LC-MS/MS
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