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目的:建立雷公藤多苷中雷公藤对醌B定性分析和含量测定方法。方法:利用高效液相色谱-电喷雾-质谱(HPLC-ESI-MS)联用结合LC-DAD技术,通过和标准化合物雷公藤对醌B的保留时间、紫外吸收光谱以及质谱中的准分子离子峰[M+Na]+相对照,快速鉴定雷公藤多苷中的雷公藤对醌B,对其含量的测定则采用了高效液相色谱方法。结果:一级质谱扫描结果表明雷公藤多苷中保留时间t R=13.2 min的峰化合物结构为雷公藤对醌B,准分子离子峰[M+Na]+为353.1,高效液相色谱结果表明雷公藤多苷中雷公藤对醌B在0.115~1.15μg呈良好的线性关系(r=0.999 9),平均回收率和RSD分别为99.32%,0.7%。结论:该方法简便、准确,可作为雷公藤多苷中雷公藤对醌B的含量测定方法。
Objective: To establish a method for the qualitative analysis and determination of quinone B in Tripterygium wilfordii. Methods: The retention time of quinone B, the UV absorption spectrum and the excimer ion in mass spectrometry were determined by high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) combined with LC-DAD technique. Peak [M + Na] + contrast, rapid identification of Tripterygium wilfordii quinone B, its content was determined by high performance liquid chromatography. Results: The results of MS-MS showed that the peak compound of tripterygium wilfordii glycosides with retention time t R = 13.2 min was tripterygium wilfordii quinone B and the quasi-molecular ion peak [M + Na] + was 353.1. The results of high performance liquid chromatography Tripterygium wilfordii Tripterygium wilfordii on quinone B in 0.115 ~ 1.15μg showed a good linear relationship (r = 0.999 9), the average recovery and RSD were 99.32%, 0.7%. Conclusion: This method is simple and accurate and can be used as a method for the determination of quinone B in Tripterygium wilfordii.