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毛细管液相色谱-微芯片-大气压光电离质谱法用于番茄中农药分析的可行性。

Feasibility of capillary liquid chromatography-microchip-atmospheric pressure photoionization-mass spectrometry for pesticide analysis in tomato.

机构信息

Institute of Chemistry, University of Tartu, Estonia.

出版信息

Anal Chim Acta. 2011 Jun 24;696(1-2):77-83. doi: 10.1016/j.aca.2011.04.006. Epub 2011 Apr 16.

Abstract

A new and sensitive analytical method, using capillary liquid chromatography (capLC) with a microfabricated heated nebulizer chip for atmospheric pressure photoionization and tandem mass spectrometry (μAPPI-MS/MS), was developed for the analysis of selected carbamate pesticides in a tomato matrix. The performance of the instrumental method was evaluated, using seven pesticides, namely oxamyl, methomyl, aldicarb, carbofuran, pirimicarb, thiocarb, and ditalimfos. The limits of detection achieved with the capLC-μAPPI-MS/MS method in the positive ion mode were low, ranging from 0.25 ng mL(-1) for pirimicarb to 5 ng mL(-1) for oxamyl and methomyl, corresponding to 5 and 0.25 μg kg(-1) for tomato samples, respectively, which are clearly below the maximum residue limits for them in fruits and vegetables. The repeatability of the instrumental method ranged from 2.9 to 13.9% (RSD) at a low (0.05 μg mL(-1)) concentration level. An adequate linearity (r(2)=0.984-0.999) at a concentration range from 0.005 to 5.0 μg mL(-1) was observed for all pesticides. The results obtained show that the capLC-μAPPI-MS/MS method developed could be used for the analysis of selected pesticides from tomato.

摘要

一种新的灵敏分析方法,使用毛细管液相色谱(capLC)与微制造加热雾化器芯片用于大气压光解和串联质谱(μAPPI-MS/MS),用于分析番茄基质中选定的氨基甲酸酯类农药。使用七种农药,即氧乐果、灭多威、涕灭威、克百威、丙溴磷、噻虫啉和丁硫克百威,对仪器方法的性能进行了评估。capLC-μAPPI-MS/MS 方法在正离子模式下的检测限较低,范围从 0.25ng mL(-1)的丙溴磷到 5ng mL(-1)的氧乐果和灭多威,分别对应于番茄样品中的 5 和 0.25μg kg(-1),明显低于水果和蔬菜中它们的最大残留限量。仪器方法的重复性在低浓度(0.05μg mL(-1))时为 2.9%至 13.9%(RSD)。在 0.005 至 5.0μg mL(-1)的浓度范围内,所有农药均表现出良好的线性(r(2)=0.984-0.999)。结果表明,所开发的 capLC-μAPPI-MS/MS 方法可用于分析番茄中的选定农药。

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