川木香药材HPLC指纹图谱及含量测定方法研究

目的:采用高效液相色谱法建立川木香药材的指纹图谱,并测定不同来源的12批川木香根茎中木香烃内酯和去氢木香内酯的含量。方法:采用WondaSil C₁₈色谱柱(4.6 mm×150 mm,5μm),以0.1%甲酸水溶液(pH 3.2)为流动相A,甲醇为流动相B,梯度洗脱,流速1 mL·min^-1,检测波长280 nm(指纹图谱建立)、254 nm(含量测定),柱温25℃,进样量10 μL。结果:以木香烃内酯为参照峰确立了40个共有峰,建立了川木香药材的HPLC指纹图谱,共有峰面积达到总峰面积90%以上,12批次药材相似度均在0.9以上;各批次药材中木香烃内酯和去氢木香内酯的含量分别在26.28~56.21 mg·g^-1和9.40~27.28 mg·g^-1之间。结论:该法经方法学验证,可为川木香药材质量分析、评价与控制提供依据。

Objective:To establish the chromatographic fingerprint of roots of Vladimiria souliei(Franch.)Ling by HPLC method,and perform the quantitative analysis of costunolide and dehydrocostuslactone in 12 batches of roots of Vladimiria souliei(Franch.)Ling.Methods:The 12 batches of samples from different producing areas were analyzed by HPLC with a Wondasil C₁₈ column(4.6 mm×150 mm,5 μm),gradient eluted with mobile phase A(water containing 0.1% formic acid,pH 3.2)-mobile phase B(methanol)at 25℃,and monitored with UV detector at 280 nm for fingerprint establishment and 254 nm for content determination.The flow rate was 1.0 mL·min^-1,and the injection volume was 10 μL.Results:Forty common peaks were selected as the fingerprint peaks with costunolide as the reference compound.The rate of common peak area to the total peak was higher than 90%,and the similarities of the correlation coefficients were higher than 0.9.The contents of costunolide and dehydrocostuslactone in different batches ranged from 26.28 to 56.21 mg·g^-1 and 9.40 to 27.28 mg·g^-1,respectively.Conclusion:This method has passed methodology validation and can provide the basis for the analysis,evaluation and control of quality of V.souliei.

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