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咖喱叶基质中采用先进质谱法的方法开发和验证:缓冲乙酸乙酯技术定量筛选 490 种多类农药。

Method development and validation in the curry leaf matrix employing advanced mass spectrometry: quantitative screening of 490 multiclass pesticides by buffered ethyl acetate technique.

机构信息

ICAR-National Research Centre for Grapes, Pune, India.

出版信息

J Environ Sci Health B. 2023;58(5):448-464. doi: 10.1080/03601234.2023.2221994. Epub 2023 Jun 18.

DOI:10.1080/03601234.2023.2221994
PMID:37332153
Abstract

Curry leaf is an evergreen herb with culinary, pharmaceutical, and nutraceutical applications. As pesticide residue in curry leaf has garnered significant regulatory attention in recent years, here we report a reliable method, which was validated for the determination of 265 and 225 pesticides using LC-MS/MS and GC-MS/MS, respectively. At first, the sample was comminuted after adding water (1:2). The sample preparation workflow included extraction of 10 g homogenized sample with 10 mL ethyl acetate (+1% acetic acid), cleanup by dispersive solid phase extraction (d-SPE, 50 mg PSA + 50 mg C + 10 mg GCB + 150 mg NaSO) and the final analysis by tandem mass spectrometry. The cleanup step adeptly removed co-extractives. The method effectively reduced matrix effects and offered an LOQ of 0.01 mg kg for most compounds. The method's accuracy and precision results fulfilled the requirements of SANTE/11312/2021 guidelines at 0.01 mg kg and higher levels of fortification. The accuracy and precision results were comparable for all pesticides. The successful screening of market samples indicates its high extraction efficiency and precision for incurred residue analysis. Due to its robustness and conformity with regulatory criteria, food testing laboratories worldwide can use the method to monitor pesticide levels in curry leaves.

摘要

咖喱叶是一种常绿草本植物,具有食用、药用和营养保健品应用价值。近年来,咖喱叶中的农药残留问题受到了广泛关注,因此我们开发了一种可靠的方法,该方法分别使用 LC-MS/MS 和 GC-MS/MS 对 265 种和 225 种农药进行了定量分析。首先,将水(1:2)加入到样品中并进行粉碎。样品制备过程包括用 10 mL 乙酸乙酯(+1% 乙酸)提取 10 g 均质化的样品,然后使用分散固相萃取(d-SPE,50 mg PSA + 50 mg C + 10 mg GCB + 150 mg NaSO)进行净化,最后通过串联质谱进行分析。净化步骤能够有效地去除共提取物。该方法有效地减少了基质效应,并为大多数化合物提供了 0.01mg/kg 的定量限(LOQ)。该方法的准确度和精密度结果在 0.01mg/kg 及以上添加水平下满足 SANTE/11312/2021 指南的要求。所有农药的准确度和精密度结果均相当。对市场样品的成功筛选表明,该方法具有较高的提取效率和残留分析精度。由于其稳健性和符合监管标准,全球食品检测实验室均可使用该方法监测咖喱叶中的农药残留水平。

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