雷公藤多苷主要有效成分的含量研究

目的: 测定雷公藤多苷中雷公藤甲素、雷公藤内酯酮、雷公藤晋碱、雷公藤次碱、雷公藤红素、雷公藤内酯甲6个有效成分的含量,为雷公藤多苷的质量评判以及组分与药效、毒性之间的关系探讨奠定基础。 方法: 采用高效液相色谱法同时测定雷公藤多苷中6个有效成分的含量,色谱柱为Agilent ZORBAX SB-C₁₈(4.6 mm×250 mm,5 μm),乙腈-0.1%磷酸-0.2%三乙胺为流动相梯度洗脱,流速0.75 mL·min^-1,柱温35℃,检测波长225 nm(0~65 min)、210 nm(65~80 min)。 结果: 在所选择的分析条件下,较好地定量了样品中的各组分。6个有效成分雷公藤甲素、雷公藤内酯酮、雷公藤晋碱、雷公藤次碱、雷公藤红素、雷公藤内酯甲的线性范围分别为0.005~0.10 mg·mL^-1(r=0.9998)、0.01~0.06 mg·mL^-1(r=0.9995)、0.10~0.20 mg·mL^-1(r=0.9993)、0.10~0.20 mg·mL^-1(r=0.9997)、0.0025~0.20 mg·mL^-1(r=0.9995)、0.015~0.07mg·mL^-1(r=0.9997);平均加样回收率为98.74%(RSD=1.5%)、96.85%(RSD=1.3%)、98.66%(RSD=2.4%)、95.61%(RSD=2.6%)、99.26%(RSD=1.9%)、99.25%(RSD=2.7%)。 结论: 所建立的方法可用于雷公藤多苷有效成分的定量分析;不同厂家生产的雷公藤多苷化学组成存在着较明显的差异。

Objective: To determine six effective components(triptolide,triptonide,wilforgine,wilforine,tripterine,wilforlide A)in tripterygium glycosides,so as to provide reference for the quality evaluation and investigation on the relationship among chemical composition,effect and toxicity. Methods: The separation was achieved using an Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm,5 μm)with an acetonitrile-0.1% phosphoric acid-0.2% triethylamine gradient elution system.The column temperature was maintained at 35℃ and the flow rate was 0.75 mL·min^-1.The elution was detected at 225 nm from 0 min to 65 min,and then at 210 nm from 65 min to 80 min. Results: Under the selected analytical condition,the components in the samples were quantified precisely.The standard curves for triptolide,triptonide,wilforgine,wilforine,tripterine and wilforlide A were linear over the ranges of 0.005-0.10 mg·mL^-1 (r=0.9998),0.01-0.06 mg·mL^-1 (r=0.9995),0.10-0.20 mg·mL^-1 (r=0.9993),0.10-0.20 mg·mL^-1 (r=0.9997),0.0025-0.20 mg·mL^-1 (r=0.9995),0.015-0.07mg·mL^-1 (r=0.9997),and the average recoveries were 98.74%(RSD=1.5%),96.85%(RSD=1.3%),98.66%(RSD=2.4%),95.61%(RSD=2.6%),99.26%(RSD=1.9%),99.25%(RSD=2.7%),respectively. Conclusion: The established method is suitable for the determination of effective ingredients in tripterygium glycosides;the differences of contents are significant among samples from different manufacturers.