雷公藤片中5种有效成分同时测定及其质量评价研究

Simultaneous determination and quality evaluation of five effective components in Tripterygium tablets

关键词:  雷公藤片  含量测定  液相色谱串联质谱法

Key words:  Tripterygium tablet  content determination  LC-MS/MS

摘要:

[目的] 建立雷公藤片中雷公藤甲素、雷公藤红素、雷公藤内酯甲、雷公藤定碱和雷酚内酯5种成分的液相色谱串联质谱法的同时定量测定的方法.[方法] 采用液相色谱质谱联用技术(ＬC-MS/MＳ)测定含量,使用Zorbax XDB-C₁₈(2.1 mm×50 mm, 3.5 μm)色谱柱,流动相采用40 mmol/L甲酸铵水溶液和0.1%甲酸甲醇溶液梯度洗脱,采用正离子模式大气压化学电离源(APCI源).检测成分的离子对质荷比分别为:雷公藤甲素(361.0/10⁵.0)、雷公藤红素(451.2/201.0)、雷公藤内酯甲(455.3/409.7)、雷公藤定碱(884.4/856.5)、雷酚内酯(313.2/225.2).[结果] 雷公藤甲素、雷公藤红素、雷公藤内酯甲、雷公藤定碱和雷酚内酯的线性关系良好(r >0.999),加样回收率分别为10⁵.67%、94.07%、101.90%、99.28%、101.92%,RSD分别为2.65%、5.17%、2.68%、2.65%、3.27%.[结论] 本研究所建立的LC-MS/MS分析方法稳定可靠、简便易行,可用于雷公藤片中雷公藤甲素、雷公藤红素、雷公藤内酯甲、雷公藤定碱和雷酚内酯5种成分的同时定量分析,为雷公藤片的质量评价和质量控制奠定了基础.

Abstract:

[Objective] To establish an LC-MS/MS method for simultaneous determination of five effective componentsof Tripterygium tablets which are: triptolide, celastrol, wilforlide A, wilfordine and triptophenolide. [Methods] The assay was performed on a Zorbax XDB-C₁₈ column(2.1 mm×50 mm, 3.5 μm) and was eluted with a mobile phase which consisted of the methonal of 0.1% formic acid and 40 mmol/L ammonium formate. 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:361.0/10⁵.0,451.2/201.0,455.3/409.7,884.4/856.5, 313.2/225.2, respectively. [Results] There was a good linear relationship over the studied concentration for the five studied components(r >0.999). The recoveries were 10⁵.67%,94.07%,101.90%,99.28%,101.92%, respectively. The RSD corresponded were 2.65%,5.17%,2.68%,2.65%,3.27%. [Conclusion] The LC-MS/MS method developed for simultaneous determination of the five effective components is simple and valid. It can be used for quality evaluation and quality control of Tripterygium tablets.