Identification and quantitation of pyrethroid pesticide residues in vegetables by solid-phase extraction and liquid chromatography/electrospray ionization ion trap mass spectrometry.
Identification and quantitation of pyrethroid pesticide residues in vegetables by solid-phase extraction and liquid chromatography/electrospray ionization ion trap mass spectrometry.
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DOI：
10.1002/rcm.3027
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发表时间：
2007-06
期刊：
影响因子：
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通讯作者：
Tianwen Chen;Guonan Chen
中科院分区：
文献类型：
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作者：
Tianwen Chen;Guonan Chen
建立了一种包括固相萃取（SPE）后接液相色谱/电喷雾电离离子阱质谱（LC/ESI - ITMS）分析的定量方法，用于蔬菜中常用的10种拟除虫菊酯类农药的鉴定和定量。采用甲醇/水混合液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，在液相色谱/质谱分析之前进行了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 - 0.1 mg/kg，相对标准偏差<20%，平均回收率为69.5% - 102.5%。所提出的方法已成功应用于6种蔬菜中拟除虫菊酯类农药的测定，结果令人满意。
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.