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[基于液相色谱-串联质谱法的六种杀菌剂快速简便分析方法的开发]

[Development of an LC-MS/MS-Based Rapid and Simple Analytical Method for Six Fungicides].

作者信息

Yoshimitsu Masato, Ueno Ryo, Matsui Hiroshi, Osakada Masakazu, Uchida Kotaro, Fukui Naoki, Akutsu Kazuhiko, Kakutani Naoya

机构信息

Osaka Institute of Public Health.

出版信息

Shokuhin Eiseigaku Zasshi. 2020;61(4):143-147. doi: 10.3358/shokueishi.61.143.

Abstract

In this study, we developed an LC-MS/MS-based rapid and simple analytical method for six fungicides; imazalil, o-phenylphenol, thiabendazole, fludioxonil, azoxystrobin and pyrimethanil, the latter three were newly approved for use after 2011. For expediting and simplification, we merged the extraction method with that of the pesticide analysis. For purification step, loading of 1 mL of sample extracts to 500 mg Oasis HLB column and elution with 8 mL of acetonitrile gave satisfactory results. The performance of the present method was confirmed for orange, grapefruit, and lemon samples fortified with the six fungicides. The results showed that the average recovery ranged from 89.7 to 100.0%, intra- and inter-assay CV% ranged from 1.5 to 5.0% and from 0.5 to 4.9%, respectively, achieving the target values of the Japanese official guideline for residual pesticide analysis. The limits of quantification of this method were determined to be 1 mg/kg for o-phenylphenol, and 0.2 mg/kg for the other five fungicides. These values were lower than their corresponding regulation values. In addition, we confirmed the usability of the present method for fungicide inspection of commercially available citrus fruits. During 2017-2019, there was no conflict between the food labeling and the fungicides detected and no fungicide with the concentration exceeding maximum residue level was detected.

摘要

在本研究中,我们开发了一种基于液相色谱-串联质谱的快速简便的六种杀菌剂分析方法,这六种杀菌剂分别是抑霉唑、邻苯基苯酚、噻菌灵、咯菌腈、嘧菌酯和嘧霉胺,后三种是2011年之后新批准使用的。为了加快分析速度并简化流程,我们将提取方法与农药分析方法合并。在净化步骤中,将1 mL样品提取物加载到500 mg的Oasis HLB柱上,并用8 mL乙腈洗脱,结果令人满意。对添加了这六种杀菌剂的橙子、葡萄柚和柠檬样品进行了本方法性能的验证。结果表明,平均回收率在89.7%至100.0%之间,批内和批间变异系数分别在1.5%至5.0%和0.5%至4.9%之间,达到了日本官方残留农药分析指南的目标值。本方法的定量限确定为邻苯基苯酚为1 mg/kg,其他五种杀菌剂为0.2 mg/kg。这些值低于其相应的规定值。此外,我们还证实了本方法可用于市售柑橘类水果的杀菌剂检测。在2017 - 2019年期间,食品标签与检测到的杀菌剂之间没有冲突,也未检测到浓度超过最大残留限量的杀菌剂。

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