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 C18反相色谱柱(50 mm×2.1 mm,1.8 μm),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0.2~50.0 μg·L-1范围内与峰面积呈线性关系,测定下限(10S/N)为0.2 μg·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 LC-MS determination. Zorbax Plus RRHD C18 column(50 mm×2.1 mm, 1.8 μm) 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 0.2-50.0 μg·L-1, with lower limit of determination (10S/N) of 0.2 μg·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 7% and 10%, respectively.