GPC-GC/MS法测定蔬菜中19种农药残留

Determination of 19 Pesticide Residues in Vegetables by Online Gel Penetration Chromatography-Microchannel Flow Technology-Gas Chromatography/Mass Spectrometry

建立了固相萃取-在线凝胶色谱-微通道气路控制-气相色谱质谱法（SPE-GPC-GCMS）测定蔬菜中农药残留的检测方法.蔬菜样品经乙腈提取,经过QuEChERS快速前处理、在线凝胶净化后,通过微通道气路控制技术（SWAFER）直接进入气相色谱质谱进行检测.色谱柱为Elite-5MS,采用程序升温进样（PSSI）,外标法定量;质谱采用SIR模式检测,离子源为EI.结果表明,农药残留在空白添加浓度5-200μg/kg范围内,峰面积与浓度呈良好的线性关系,相关系数均大于0.990;总体回收率在65.1-140%之间;方法的检出限为0.5-5.0μg/kg.

A method for determination of pesticide residues in vegetables by online gel filtration chromatography-gas chromatography/mass spectrometry （GPC-GC/MS） was established. Pesticide residues in vegetable samples were ex-tracted with acetonitrile, purified by QuEChERS and online GPC, injected with programmable temperature increase through a SWAFER into the gas chromatograph-mass spectrometer, separated on an Elite-5MS column, detected under the SIR mode using an EI source and quantified by external standard method. Good linearity between peak areas and concentrations was demonstrated over the concentration range of 5-200μg/kg; the correlation coefficient was greater than 0.990 for all analytes. The recoveries were between 65.1% and 140%. The limits of detection were between 0.5 and 5.0μg/kg.