中国临床药学杂志

目的建立一种灵敏、准确的雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量的LC-MS法。方法雷公藤浸膏样品经氯仿溶解后用稀盐酸(2.0 mol·L^-1)溶液提取,上清液移入Oasis(?)MCX固相萃取小柱进行净化,然后样品在Zorbax Plus RRHD C₁₈柱(50 mm×2.1 mm,1.8μm)上,以醋酸铵缓冲液[0.05%醋酸-酸酸铵溶液(5 mmol·L^-1)]-乙腈(30:70)为流动相进行分离,应用LC-MS法,在大气压化学电离正离子选择离子监测模式(SIM)下测定,雷公藤新碱和雷公藤碱戊的定量离子分别为m/z806和m/z 779。结果雷公藤新碱和雷公藤碱戊的绝对回收率为87.0%~97.5%,在含量1.0~200.0μg·kg^-1内均具有良好线性,日内RSD均<9.8%,日间RSD均<14.7%,定量检出限均为1.0μg·kg^-1。结论本方法简便、灵敏、干扰少、特异性好,可用于雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量的监测。

AIM To establish a sensitive and accurate method for the determination of contents of trace euonine and wilforidine in Tripterygium wUfordii hook.F.extract by liquid chromatography coupled with mass spectrometry(LCMS).METHODS After the alkaloids in Tripterygium wUfordii hook.F.extract was dissolved by chloroform and extracted by hydrochloric acid solution(2.0 mol·L^-1),the supernatant was cleaned by the solid-phase extraction(SPE)using Oasis(?) MCX cartridges.The separation was performed on a Zorbax Plus RRHD C₁₈ column(50 mm× 2.1 mm,1.8 μm)using a mobile phase consisting of 0.05%acetic acid-ammonium acetate(5 mmol·L^-1)-acetonitrile(30:70).Detection was carried out by a positive atmospheric-pressure chemical ionization mass spectrometry(APCI-MS) in the selected ion monitoring(SIM) mode with the protonated molecular ions m/z 806[M + H]⁺ and m/z 779[M + H]⁺ for euonine and wilforidine,respectively.RESULTS Calibration curves were linear within the range of 1.0-200.0 μg· kg^-1,and the extraction recoveries were from 87.0%to 97.5%.The intra-day RSD was less than 9.8%,the inter-day RSD was less than 14.7%,and the limits of quantification(LOQ) were 1.0μg·kg^-1 for the two alkaloids.CONCLUSION This method is found to be simple,sensitive and little interferential,and can be used for the determination of trace euonine and wilforidine in Tripterygium wilfordii hook.F.extract.