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作 者:何昱[1] 石森林[1] 张茹萍[1] 钱家健[1] 范永升[1]
出 处:《药物分析杂志》2013年第2期197-200,共4页Chinese Journal of Pharmaceutical Analysis
基 金:浙江省重点科技创新团队项目(2011R09042-06);浙江省教育厅科研项目(Y201120445)
摘 要: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,5μm),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 Agi- lent ZORBAX SB -C18 column(4. 6 mm ×250 mm,5 /zm) with an acetonitrile -0. 1% phosphoric acid -0. 2% tri- ethylamine 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. Re- stilts : Under the selected analytical condition, the components in the samples were quantified precisely. The standard cur ves for triptolide, triptonide, wilforgine, wilforine, tripterine and wilforlide A were linear over the ranges of 0. 005 - 0. 10 nag · mL^ - 1 ( r = 0. 9998 ), 0. 01 - 0. 06 mg · mL ^- 1 ( r = 0. 9995 ), 0. 10 - 0. 20 mg · naL ^- 1 ( r = 0. 9993 ), 0.10-0.20 nag· mL^-1(r=0.9997),0.0025-0.20 mg · naL^-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 differ- ences of contents are significant among samples from different manufacturers.
关 键 词:雷公藤多苷 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 高效液相色谱法
分 类 号:R917[医药卫生—药物分析学]
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