高效液相色谱-串联质谱法测定药食同源中药材中29种农药残留

Determination of 29 pesticide residues in medicinal and edible traditional chinese medicine by high performance liquid chromatography-tandem mass spectrometry

建立了固相萃取-高效液相色谱-串联质谱法测定药食同源中药材中29种农药的分析方法。样品用乙腈提取,固相萃取柱净化,经Agilent poroshell 120 EC-C_(18)色谱柱(100 mm×3.0 mm,2.7μm)分离,质谱采用电喷雾电离源,多反应监测模式检测,以色谱峰面积外标法定量。29种农药质量浓度与色谱峰面积线性相关,相关系数为0.995~0.999 4,检出限为0.002~0.05 mg/kg,高、中、低3个不同浓度加标回收率为79.5%~108.7%,相对标准偏差为3.05%~6.71%(n=6)。该方法降低了药食同源样品中基质干扰,方法准确、快速,可用于大批量样品中农药残留的检测分析。

An analytical method was established for the determination of 29 pesticide residues in medicinal and edible traditional chinese medicines by solid phase extraction high performance liquid chromatography tandem mass spectrometry.The sample was extracted with acetonitrile,and then purified by solid phase extraction column,then the sample was separated by Agilent poroshell 120 EC-C_(18)chromatography column(100 mm×3.0 mm,2.7 μ m),and the mass spectrum of the sample was detected by the multi reaction monitoring mode with an electrospray ionization source,and quantified by the chromatographic peak area external standard method.The mass concentration of 29 pesticides were linearly correlated with the chromatographic peak area,the linear correlation coefficients were 0.995-0.999 4,and the detection limits of this method were 0.002-0.05mg/kg.The average recoveries ranged from 79.5% to 108.7% at the three spiked levels,and the relative standard deviations were in the range of 3.05%-6.71%(n=6).This method reduces the matrix interference in the medicinal and edible samples,which is accurate and rapid,ans it can be used for the detection and analysis of pesticide residues in a large number of samples.