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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 C_(18)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。
Objective To establish a sensitive and accurate LC-MS method for the determination of triptolide and tripterygium pentane in Tripterygium wilfordii extract. Methods Tripterygium wilfordii extract samples were dissolved in chloroform and extracted with dilute hydrochloric acid (2.0 mol·L -1). The supernatant was transferred to Oasis MCX solid phase extraction cartridges for purification. The samples were then separated on a Zorbax Plus RRHD (50 mmol x L (-1))] - acetonitrile (30:70) on a C 18 column (50 mm × 2.1 mm, 1.8 μm) The mobile phase was separated and the quantitation ions of triptolide and tripterygium wilfordii were m / z 806 and m / z 779, respectively, using LC-MS method under atmospheric pressure chemical ionization positive ion selective ion monitoring mode (SIM) . Results The absolute recoveries of triptolide and tripterygium wilfordii were 87.0% -97.5%, with good linearity in the range of 1.0-200.0 μg · kg -1. The intra-day RSD was less than 9.8%, and the intraday RSD All <14.7%, the limit of quantification was 1.0μg · kg ~ (-1). Conclusion The method is simple, sensitive, less perturbed and has good specificity. It can be used to monitor the contents of triptolide and triptolide in Tripterygium wilfordii extract.