固相萃取-高效液相色谱-串联质谱法测定中药西南金丝梅中26种农药残留量  

HPLC-MS/MS Determination of Residual Amounts of 26 Pesticides in TCM Hypericum Augustinnii N. Robson with Solid-Phase Extraction

作　　者：胡晓旭[1] 杨宏兴 熊佳梁 谭伟[1] 王红斌[1] 杨敏[1] 

机构地区：[1]云南民族大学化学与生物技术学院,民族药资源化学国家民族事务委员会-教育部重点实验室,昆明600500 [2]云南省农业环境保护监测站,昆明650034 [3]大理州农产品质量安全监督检验测试中心,大理671005

出　　处：《理化检验（化学分册）》2013年第6期661-665,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：民族药资源化学国家民委-教育部重点实验室开放基金(MZY1121);大学生创新性实验项目(11HXYJSZ1)

摘　　要：提出了高效液相色谱-串联质谱法测定西南金丝梅中26种农药残留量的方法。样品用乙腈振荡提取,提取液经氨基固相萃取小柱净化。用shim-packXR-ODS色谱柱分离,采用电喷雾离子化正离子方式及多反应监测模式进行测定。26种农药的质量浓度在0.01～2.5mg·L-1范围内与峰面积呈线性关系,检出限(3S/N)在4.16×10-5～2.85×10-4 mg·kg-1之间。在3个标准加入水平下进行了精密度和回收试验,方法的回收率在78.4%～112%之间,测定值的相对标准偏差(n=5)在1.2%～11%之间。A method of HPLC-MS/MS for the determination of residual amounts of 26 pesticides in hypericum augustinnii N. Robson was proposed.The sample was extracted oscillatorily with acetonitrile,and the extract was purified by NH2-solid phase extraction column.Shim-packXR-ODS column was used as chromatographic column,and positive electrospray ionization as well as multiple reactions monitoring mode was used in the detection.Linear relationships between values of peak area and mass concentration of 26 pesticides were kept in the range of 0.01-2.5 mg·L-1,with detection limits（3S/N） in the range of 4.16×10-5-2.85×10-4mg·kg-1.Tests for recovery and precision were made by addition of standard solution at 3 different concentration levels,which were then analyzed by the proposed method.Values of recovery found were in the range of 78.4%-112%,and values of RSD′s（n=5） found were in the range of 1.2%-11%.

关 键 词：固相萃取 高效液相色谱-串联质谱法 农药 西南金丝梅 

分 类 号：O652.63[理学—分析化学]