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采用固相萃取和液相色谱/电喷雾电离离子阱质谱法鉴定和定量蔬菜中的拟除虫菊酯类农药残留

Identification and quantitation of pyrethroid pesticide residues in vegetables by solid-phase extraction and liquid chromatography/electrospray ionization ion trap mass spectrometry.

作者信息

Chen Tianwen, Chen Guonan

机构信息

Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, Fujian, 350002, China.

出版信息

Rapid Commun Mass Spectrom. 2007;21(12):1848-54. doi: 10.1002/rcm.3027.

Abstract

A quantitative method consisting of solid-phase extraction (SPE) followed by liquid chromatography/electrospray ionization ion trap mass spectrometry (LC/ESI-ITMS) analysis was developed for the identification and quantitation of ten pyrethroid pesticides commonly used in vegetables. The best HPLC separation was achieved using a gradient program of methanol/water mixture. For the vegetable samples, an SPE procedure to clean up the matrices was carried out prior to LC/MS analysis. Under the optimum conditions, the limits of quantification of the pyrethroid pesticides (tetramethrin, allethrin, fenpropathrin, lambda-cyhalothrin, cypermethrin, deltamethrin, fenvalerate, bioresmethrin, permethrin and bifenthrin) ranged from 0.03 to 0.1 mg kg-1 with relative standard deviations<20%, and the mean recoveries ranged from 69.5 to 102.5%. The proposed method has been successfully applied to the determination of pyrethroids in six vegetables with satisfactory results.

摘要

建立了一种定量方法,该方法包括固相萃取(SPE),然后进行液相色谱/电喷雾电离离子阱质谱(LC/ESI-ITMS)分析,用于鉴定和定量蔬菜中常用的十种拟除虫菊酯类农药。使用甲醇/水混合物的梯度程序实现了最佳的高效液相色谱分离。对于蔬菜样品,在进行液相色谱/质谱分析之前,先进行固相萃取程序以净化基质。在最佳条件下,拟除虫菊酯类农药(胺菊酯、丙烯菊酯、甲氰菊酯、高效氯氟氰菊酯、氯氰菊酯、溴氰菊酯、氰戊菊酯、苄呋菊酯、氯菊酯和联苯菊酯)的定量限为0.03至0.1 mg kg-1,相对标准偏差<20%,平均回收率为69.5至102.5%。该方法已成功应用于六种蔬菜中拟除虫菊酯类农药的测定,结果令人满意。

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