人参中农药多残留的超高效液相色谱-串联质谱分析方法研究

以传统中药人参为研究对象, 建立一种同时检测人参中46 种农药多残留的基质固相分散-超高效液相色谱-串联质谱(MSPD-UPLC-MS/MS)方法. 前处理方法分别采用N-丙基乙二胺(PSA)和乙腈作为MSPD的分散剂和洗脱剂, 检测方法采用正负离子同时扫描, 利用超高效液相色谱-串联质谱在分时段多反应监测模式下进行定量和定性分析. 大部分农药在5～500 μg/kg 范围内线性关系良好, 在低(10 μg/kg)、中(50 μg/kg)、高(100 μg/kg)三个浓度水平上的添加回收率平均值在70%～110%之间, 相对标准偏差(RSD)小于15% (n＝3), 定量限小于0.01 mg/kg, 能够满足农药多残留分析要求. 该方法通用性强、选择性好、灵敏度高、简单廉价.

Studies on the Determination Method of Pesticide Multi-residues in Ginseng by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

Taking the traditional herbal,ginseng,as the object in the paper,a comprehensive analytical method based on matrix solid-phase dispersion-ultra performance liquid chromatography tandem mass spec-trometry(MSPD-UPLC-MS/MS) has been developed for the simultaneous determination of 46 pesticide residues in Ginseng.The sample was prepared by MSPD.Primary secondary amine(PSA) was used as dis-persant,and acetonitrile was used as eluant.Both positive and negative ionization modes were used in the detection.Qualitative and quantitative analysis was carried out by UPLC-MS/MS under multiple reaction monitoring mode(MRM).The linear range of this method was 5～500.0 μg/kg.The limits of quantification(LOQ) for the 46 pesticides were less than 0.01 mg/kg.The mean recoveries at the three spiked levels of 10～100 μg/kg were 70%～110%,with relative standard deviations(RSD) better than 15%(n=3).The method is robust,selective,sensitive,rapid and cheap.