提出了尿液中雷公藤春碱的高效液相色谱-质谱测定方法。尿液样品经Waters Oasis MCX固相萃取小柱富集、净化后,以Zorbax Eclipse SB C18反相色谱柱(4.6 mm×250 mm,5 μm)为分离柱,以乙酸盐缓冲溶液-乙腈(40+60)为流动相,采用正离子模式大气压化学电离源,在选择离子监测模式下进行检测,雷公藤春碱的定量离子质荷比(m/z)为874.4。线性范围为0.2~50.0 μg·L-1,检出限(3S/N)为0.07 μg·L-1,测定下限(10S/N)为0.2 μg·L-1。回收率在86.0%~92.0%之间,日内(n=6)和日间(n=15)相对标准偏差分别小于7.5%和10.5%。

A method for the determination of wilfortrine in urine by HPLC-MS was proposed. Wilfortrine in sample was separated, enriched and purified on the Waters Oasis MCX SPE column. The eluate was used for HPLC-MS determination, in which the Zorbax Eclipse SB C18 column (4.6 mm×250 mm, 5 μm) was used as chromatographic column, and a mixture of acetate buffer solution and acetonitrile (40+60) was used as mobile phase. Atmospheric pressure chemical ionization source with positive ionization mode as well as selected ion monitoring mode was used in the detection. Ion used for quantification was m/z 874.4. Linearity range was found between 0.2-50.0 μg·L-1, and values of detection limit (3S/N) and lower limit of determination (10S/N) found were 0.07 μg·L-1 and 0.2 μg·L-1 respectively. Values of recovery were ranged from 86.0% to 92.0%. Values of RSD′s (intra-day, n=6) and RSD′s (inter-day, n=15) were less than 7.5% and 10.5%, respectively.