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LC-MS/MS 法分析西瓜中多类农药残留

Residue analysis of multi-class pesticides in watermelon by LC-MS/MS.

机构信息

Department of Chemistry and Research Institute of Life Science, Gyeongsang National University, Jinju, Republic of Korea.

出版信息

J Sep Sci. 2010 Mar;33(4-5):493-501. doi: 10.1002/jssc.200900644.

Abstract

As watermelon is farmed primarily by protected and successive cultivation techniques, a number of pesticides are required for the control of pests and diseases. To evaluate the harmful effects of pesticides in watermelon and to guarantee consumers' safety, a rapid screening process for pesticides is required. A LC-MS/MS method was applied for the direct quantitation of 44 pesticide residues in watermelon. A Zorbax XDB-C(18) column was selected for analysis, with a mobile phase consisting of a gradient system of water and 5 mM methanolic ammonium formate. MS/MS experiments were performed in ESI positive ion and multiple reaction monitoring modes. The LOQs were in the range of 1-26 microg/kg, thereby indicating good sensitivity. Most of the recoveries ranged between 70-131% with RSDs < or = 20%. We suggested that the amount of pesticide residues such as pyroquilon (pyn), boscalid (bd), and dimethomorph (di) in amides (AM) and cinosulfuron (ci) in ureas (UR) may have been overestimated for the pesticides owing to increased alpha-error risk, whereas the amounts of pesticide residues, such as imibenconazole (ie) in the triazoles (TR) and fenpyroximate (fee) in the imidazoles (IM), may have been underestimated as the result of increased beta-error risk. The current method allowed for the rapid quantitation and identification of low pesticide levels in the watermelon samples. No pesticide residues were detected in any of the surveyed watermelons obtained from eight local markets in the Republic of Korea. Statistical analysis of the recoveries classified the 44 pesticides into nine groups and three overall categories.

摘要

由于西瓜主要采用保护和连续的栽培技术,因此需要使用多种农药来防治病虫害。为了评估农药对西瓜的有害影响,保障消费者的安全,需要快速筛选农药。本研究应用 LC-MS/MS 法直接定量分析了西瓜中的 44 种农药残留。选用 Zorbax XDB-C(18)柱进行分析,流动相由水和 5mM 甲醇甲酸铵组成的梯度系统组成。采用电喷雾正离子多反应监测模式进行 MS/MS 实验。LOQs 范围为 1-26μg/kg,表明具有良好的灵敏度。大多数回收率在 70-131%之间,RSDs<20%。我们建议,由于增加了 alpha 错误风险,酰胺类(AM)中的吡喹酮(pyn)、苯醚甲环唑(bd)和二甲噻菌胺(di)以及脲类(UR)中的嘧啶肟菌酯(ci)的农药残留量可能被高估,而三唑类(TR)中的咪鲜胺(ie)和咪唑类(IM)中的氟啶虫酰胺(fee)的农药残留量可能由于增加了 beta 错误风险而被低估。本方法能够快速定量和鉴定西瓜样品中的低水平农药残留。在所调查的韩国 8 个本地市场购买的西瓜样品中均未检测到农药残留。对回收率进行的统计分析将 44 种农药分为 9 组和 3 个总体类别。

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