气相色谱-三重四极杆串联质谱法同时测定太子参中34种农药残留

Simultaneous Determination of 34 Pesticide Residues in Pseudostellariae Radix by Gas Chromatography-triple Quadrupole Tandem Mass Spectrometry

关键词:  太子参  农药残留  快速样品处理技术  气相色谱-三重四极杆串联质谱

Key words:  Pseudostellariae Radix  pesticide residues  QuEChERS  GC-MS/MS

摘要:

目的 采用快速样品处理技术（QuEChERS）结合气相色谱-三重四极杆串联质谱（GC-MS/MS）建立太子参中34种农药残留同时检测的方法。方法 样品用乙腈提取，经过分散固相萃取柱净化后，在GC-MS/MS于多反应监测模式下进行检测，采用基质匹配标准曲线内标法进行定量，以3个添加水平测定样品的回收率和RSD。结果 各农药线性关系良好，相关系数均>0.997，仪器精密度RSD为0.3%~4.8%，回收率为70.6%~106.9%，重复性RSD为2.2%~7.4%，检测限均<0.005 mg·kg^-1。结论 该方法简便、灵敏、准确、可靠，可用于太子参中34种农药残留的测定。

Abstract:

OBJECTIVE To establish a method for the simultaneous determination of 34 pesticide residues in Pseudostellariae Radix with combination of QuEChERS and gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). METHODS Sample was extracted with acetonitrile, and the extract was further purified by dispersive solid-phase extraction. The prepared sample was analyzed by GC-MS/MS in multi-reaction monitoring mode and matrix-matched internal standard method was applied to quantify the pesticides. There were three supplemental levels for determing rates of recovery and RSD. RESULTS All pesticides had good linearity with correlation coefficient higher than 0.997. The RSD of instruments precision were 0.3%-4.8%. The rates of recovery were 70.6%-106.9%, and the RSD of repeatability were 2.2%-7.4%. The limits of detection all<0.005 mg·kg^‒1.CONCLUSION The method is simple, sensitive, accurate and reliable, and it can be used for the determination of 34 pesticide residues in Pseudostellariae Radix.