液相色谱-串联质谱法测定人参中申嗪霉素的残留

摘要

A liquid chromatography coupled with electrospray ionization tandem mass spectrometric ( LC-MS/MS )method was developed for the determination of phenazine-1-carboxylic acid in gin-seng. The ginseng samples were soaked with water,extracted with acetonitrile and cleaned-up by dispersive solid-phase extraction,separated by chromatography,then detected by MS/MS under mul-tiple reaction monitoring( MRM)mode via positive electrospray ionization. The ion-pair of 225. 1/179. 1 was used for quantitative analysis,and the ion-pair of 225. 1/125. 1 was selected for qualita-tive analysis. The external standard method was used for the quantification analysis. The limit of quantitation( LOQ)of phenazine-1-carboxylic acid was 0. 01 mg/kg. The standard calibration curve was linear in the range of 0. 5-10 μg/L,with correlation coefficient more than 0. 99. The recover-ies of phenazine-1-carboxylic acid in ginseng were in the range of 82% -100% at three spiked levels of 0. 01,0. 02 and 0. 10 mg/kg,with relative standard deviations( RSDs)not more than 6. 8% . The result showed that the method was simple,rapid and highly sensitive,and could be applied in the determination of phenazine-1-carboxylic acid in ginseng.%建立了液相色谱-电喷雾串联质谱测定人参中申嗪霉素残留量的分析方法。人参样品经水浸泡，乙腈提取，分散固相萃取净化，色谱分离后，采用ESl-MS/MS在正离子多反应监测（ MRM）模式下进行检测，选择定量离子对为m/z 225.1/179.1，定性离子对为m/z 225.1/125.1，外标法定量。该方法对于人参中申嗪霉素的定量下限为0.01 mg/kg，在0.5~10μg/L质量浓度范围内，峰面积与含量呈良好线性关系，相关系数大于0.99。对人参中申嗪霉素在0.01，0.02，0.10 mg/kg加标水平下的回收率为82％~100％，相对标准偏差均不大于6.8％。结果表明，该方法操作简单、快速，灵敏度和准确度高，可满足人参中申嗪霉素残留量的检测要求。