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[使用液相色谱-串联质谱法对绿茶中农药残留改进的多残留方法进行单实验室验证研究]

[Single-laboratory Validation Study of an Improved Multi-residue Method for Pesticide Residues in Green Tea Leaves Using LC-MS/MS].

作者信息

Takada Tomomi, Tomizawa Sanae, Fujiwara Takushi, Kamijo Kyoko, Yamamoto Kazuoki, Saito Yuri, Kokaji Yoshie, Ohsawa Yoshihiro, Noguchi Maiko, Tahara Shoichi

机构信息

Tokyo Metropolitan Institute of Public Health.

出版信息

Shokuhin Eiseigaku Zasshi. 2025;66(3):56-60. doi: 10.3358/shokueishi.66.56.

Abstract

In this study, a multi-residue method for pesticide residues in green tea leaves was developed using LC-MS/MS and the validity of the developed method was evaluated in accordance with Japanese guidelines. Based on the previously reported method, the amount of acetonitrile used for extraction, amount of hexane-washed distilled water added to the sample, and solid-phase column used for purification were investigated. In the developed method, the pesticides were extracted with 25 mL of acetonitrile after adding 10 mL of the hexane-washed distilled water to the sample and salted out. By cleaning the acetonitrile layer using Inert Sep PLS-3 (200 mg/20 mL) and SupelcleanENVI-CarbII/PSA (300 mg, 600 mg/6 mL), the effect of the matrix on the green tea leaves was reduced. This method was validated by performing recovery tests at two concentrations (0.01 and 0.1 mg/kg) of 92 pesticides. Of the 92 pesticides, 84 met the criteria. The limit of quantification was 0.01 mg/kg, which is the uniform limit specified by the Food Sanitation Law of Japan. This study presents that the developed method is useful for the analysis of pesticide residues in green tea leaves.

摘要

在本研究中,使用液相色谱 - 串联质谱法(LC-MS/MS)开发了一种用于测定绿茶叶片中农药残留的多残留方法,并根据日本指南对所开发方法的有效性进行了评估。基于先前报道的方法,研究了用于提取的乙腈用量、添加到样品中的己烷洗涤蒸馏水的量以及用于净化的固相柱。在所开发的方法中,向样品中加入10 mL己烷洗涤蒸馏水并盐析后,用25 mL乙腈提取农药。通过使用Inert Sep PLS-3(200 mg/20 mL)和Supelclean ENVI-CarbII/PSA(300 mg,600 mg/6 mL)净化乙腈层,减少了基质对绿茶叶片的影响。通过对92种农药在两种浓度(0.01和0.1 mg/kg)下进行回收率测试,验证了该方法。在这92种农药中,有84种符合标准。定量限为0.01 mg/kg,这是日本《食品卫生法》规定的统一限量。本研究表明,所开发的方法可用于分析绿茶叶片中的农药残留。

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