雷公藤多苷中雷公藤对醌B的LC-MS定性和HPLC定量分析

Determination of Triptoquinone B in Tripterygium Glycosides by LC-MS Analysis and HPLC

摘要:

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0.115~1.15 μg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。

Abstract:

Objective: To develop an analytic method for determination of triptoquinone B in tripterygium glycosides. Method: The HPLC-ESI-MS and HPLC-DAD methods were established. Triptoquinone B in tripterygium glycosides was quickly identified by comparing the retention time, UV absorption spectrum and quasi-molecular ion peak [M+Na]⁺ with the reference compound. The content of triptoquinone B in tripterygium glycosides was determined by HPLC. Result: One level mass spectrometry scanning results showed that the chromatographic peak of retention time t_R=13.2 min was identified as triptoquinone B, and its quasi-molecular ion peak [M+Na]⁺ was 353.1.The calibration curves of triptoquinone B was linear between 0.115-1.15 μg (r=0.999 9). The average recovery and the relative standard deviation were 99.32% and 0.7% respectively. Conclusion: The method is simple, accurate and could be used for determination of triptoquinone B in tripterygium glycosides.