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采用固相萃取和液相色谱-质谱联用技术测定蔬菜和水果中的新烟碱类农药残留量。

Determination of neonicotinoid pesticide residues in vegetables and fruits with solid phase extraction and liquid chromatography mass spectrometry.

作者信息

Obana Hirotaka, Okihashi Masahiro, Akutsu Kazuhiko, Kitagawa Yoko, Hori Shinjiro

机构信息

Osaka Prefectural Institute of Public Health, 1-3-69 Nakamichi, Higashinari, Osaka 5370025, Japan.

出版信息

J Agric Food Chem. 2003 Apr 23;51(9):2501-5. doi: 10.1021/jf0261102.

DOI:10.1021/jf0261102
PMID:12696927
Abstract

A rapid and simple extraction method for the simultaneous analysis of five neonicotinoid insecticides has been developed. Twelve different fruit and vegetable matrixes were extracted with methanol and cleaned up using a graphitized carbon solid phase extraction cartridge loading with a 20% methanol solution. The concentrated eluate after methanol elution was then analyzed for pesticide residues by liquid chromatography/mass spectrometry in the APCI positive mode. The five pesticides including nitenpyram, thiamethoxam, imidacloprid, acetamiprid, and thiacloprid were recovered at 70-95% at spike levels of 0.1 and 1 mg/kg in bell pepper, cucumber, eggplant, grape, grapefruit, Japanese radish, peach, pear, potato, rice, and tomato. Relative standard deviations were less than 10% for all of the recovery tests. The proposed method is fast, easy to perform, and could be utilized for regular monitoring of pesticide residues.

摘要

已开发出一种快速简便的提取方法,用于同时分析五种新烟碱类杀虫剂。用甲醇提取十二种不同的果蔬基质,并用装填20%甲醇溶液的石墨化碳固相萃取柱进行净化。甲醇洗脱后的浓缩洗脱液然后通过液相色谱/质谱在大气压化学电离正模式下分析农药残留。在甜椒、黄瓜、茄子、葡萄、柚子、白萝卜、桃子、梨、土豆、大米和番茄中,啶虫脒、噻虫嗪、吡虫啉、啶虫脒和噻虫啉这五种农药在0.1和1 mg/kg的加标水平下回收率为70-95%。所有回收率测试的相对标准偏差均小于10%。所提出的方法快速、易于操作,可用于农药残留的常规监测。

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