藏药六味木香丸的定性定量检测方法研究

On the Qualitative and Quantitative Detection Methods of Tibetan Medicine Liuwei Muxiang Wan

目的:建立藏药六味木香丸的定性定量检测方法,为质量标准修订提供参考。方法:采用TLC法对藏药六味木香丸中木香、石榴子、余甘子和荜茇进行定性鉴别;采用HPLC法测定藏药六味木香丸中木香烃内酯和去氢木香烃内酯的含量,使用C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-水(65∶35)为流动相,流速1.0 m L·min-1,检测波长225 nm,柱温25℃。结果:薄层色谱斑点清晰,分离度良好,阴性样品无干扰。木香烃内酯质量浓度在12~60μg·m L-1范围内线性关系良好(r=0.9997),平均回收率(n=6)为98.8%,RSD=1.6%;去氢木香烃内酯质量浓度在17~85μg·m L-1范围内线性关系良好(r=0.9996),平均回收率(n=6)为99.8%,RSD=1.4%。结论:所建立的方法准确、可靠,专属性强,可用于六味木香丸的质量控制。

Objective： To establish the qualitative and quantitative detection methods for Tibetan Medicine Liuwei Muxiang Wan. Methods： TLC was used to identify Radix Aucklandiae, Pomegranate seed, Phyllanthi Fructus, and Piperis Longi Fructus. HPLC method was used to determine costunolide and dehydrocostuslactone in Tibetan Medicine Liuwei Muxiang Wan. The procedure was performed on an Agilent 5 TC-C18 column（4.6 mm×250 mm, 5 μm） at 25℃, with acetonitrile-water（65∶35） as mobile phase and the detection wavelength was set at 225 nm. Results： The clear TLC spots showed good resolution without interference from negative samples. The calibration curve of costunolide was linear in the mass concentration range of 12-60 μg·m L-1（r = 0.9997）, and the average recovery rate was 98.8% with the corresponding RSD of 1.6%; the calibration curve of dehydrocostuslactone was linear in the mass concentration range of 17-85 μg·m L-1（r = 0.9996）, and the average recovery rate was 99.8% with the corresponding RSD of 1.4%. Conclusion： The established method of identification is accurate, simple and specific, and can be used in the quality control of Liuwei Muxiang Wan.