液相色谱-质谱法测定人尿中雷公藤新碱含量  

LC-MS Determination of Euonine in Human Urine

作　　者：沈称意[1] 施跃锦[1] 蔡美强[1] 金米聪[2] 

机构地区：[1]浙江工商大学环境科学与工程学院,杭州310035 [2]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,宁波315010

出　　处：《理化检验（化学分册）》2013年第7期773-776,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江省公益性技术应用研究计划项目(2011C37002);宁波市自然科学基金项目(2011A610058)

摘　　要：提出了人尿中雷公藤新碱的液相色谱-质谱测定方法。尿液样品经Waters Oasis MCX固相萃取柱富集并净化,萃取柱用含氨水的乙腈洗脱。洗脱液用Zorbax Plus RRHD C_(18)反相色谱柱(50 mm×2.1 mm,1.8μm),以乙酸盐缓冲溶液和乙腈(30+70)混合液为流动相进行分离,采用大气压化学电离源正离子模式在选择离子监测模式下进行检测,雷公藤新碱的定量离子为m/z 806。雷公藤新碱的质量浓度在0.2~50.0μg·L^(-1)范围内与峰面积呈线性关系,测定下限(10S/N)为0.2μg·L^(-1)。回收率在84.5%~94.0%之间,日内(n=6)和日间(n=5)精密度分别小于7%和10%。A method for the determination of euonine in human urine by LC-MS was proposed. Euonine in sample was separated, enriched and purified on Waters Oasis MCX SPE column. The SPE column was eluted with ammoniacal acetonitrile. The eluate was used for LCMS determination. Zorbax Plus RRHD C18column（50 mm×2.1mm,1.8μm） was used as chromatographic column, and a mixture of acetate buffer solution and acetonitrile （30＋70） was used as mobile phase in the separation. Atmospheric pressure chemical ionization source with positive ionization mode as well as selected ion monitoring mode was used in the detection. Quantitative ion of euonine used was m/z 806. Linear relationship between values of peak area and mass concentration of euonine was kept in the range of 0. 2 50.0μg·L^-1 , with lower limit of determination （10S/N） of 0.2μg·L^-1. Values of recovery were ranged from 84.5% to 94.0%. Values of intraday RSD＇s （n=6） and interday RSD＇s （n=5） found were less than 70/oo and 10%, respectively.

关 键 词：液相色谱-质谱法 固相萃取 雷公藤新碱 尿液 

分 类 号：O657.7[理学—分析化学]