蒙药泡囊草的定性鉴别及含量测定

目的：建立泡囊草的鉴别及含量测定方法。方法：以硅胶G为吸附剂，乙酸乙酯-甲醇（13：2）为展开剂，在紫外灯（365 nm）下观察，对香豆素-7-O-β-D-葡萄糖苷进行薄层色谱鉴别；以硅胶G为吸附剂，乙酸乙酯-甲醇-氨试液（17：3：1）为展开剂，改良碘化铋钾溶液为显色剂，对东莨菪碱进行薄层色谱鉴别。以香豆素-7-O-β-D-葡萄糖苷、6-甲氧基香豆素-7-O-β-D-葡萄糖苷、东莨菪碱和莨菪碱为指标，采用C₁₈色谱柱（250 mm×4.6 mm，5 μm），以乙腈-醋酸钠缓冲液（pH 6.0）（15：85）为流动相，流速1.0 mL·min^-1，检测波长257 nm，对不同来源泡囊草进行含量测定。结果：泡囊草薄层色谱鉴别斑点清晰，易于鉴别；在本研究所采用的高效液相色谱条件下，所有香豆素-7-O-β-D-葡萄糖苷、6-甲氧基香豆素-7-O-β-D-葡萄糖苷、东莨菪碱和莨菪碱质量浓度分别在50~250、20~100、50~250、20~100 μg·mL^-1范围内线性关系良好（r>0.999 5），平均回收率分别为96.8%、97.5%、97.8%、96.5%，不同来源的5批样品中上述4个化合物平均含量变化分别为（1.271±0.045）、（0.407±0.035）、（0.906±0.044）和（0.325±0.036）mg·g^-1。结论：建立的泡囊草定性和定量分析方法，为综合评价该药材质量提供依据。

Objective:To develop identification and quantitation methods for roots of Physochlaina phsaloides.Methods:Coumarin-7-O-β-D-glucoside was identified by TLC with silica gel G as the stationary phase and ethyl acetate-methanol (13:2) as developing solvent.The spot was detected under ultraviolet light at 365 nm.Scopolamine was identified by TLC with silica gel G as the stationary phase,ethyl acetate-methanol-ammonia water (17:3:1) as developing solvent and modified Dragendorff's solution as chromogenic reagent.Coumarin-7-O-β-D-glucoside,6-methoxylcoumarin-7-O-β-D-glucoside,scopolamine and hyoscyamine were determined by HPLC with C₁₈ column (250 mm×4.6 mm,5 μm) as stationary phase,acetonitrile-sodium acetate buffer (pH 6) (15:85) as mobile phase at a flow rate of 1.0 mL·min^-1.Detection wavelength was set at 257 nm.Results:The TLC spots were clear and easy to be identified.The calibration curves were linear within the range of 50-250 μg·mL^-1 for coumarin-7-O-β-D-glucoside,20-100 μg·mL^-1 for 6-methoxylcoumarin-7-O-β-D-glucoside,50-250 μg·mL^-1 for scopolamine and 20-100 μg·mL^-1 for hyoscyamine (r>0.999 5).The recoveries of coumarin-7-O-β-D-glucoside,6-methoxylcoumarin-7-O-β-D-glucoside,scopolamine and hyoscyamine were 96.8%,97.5%,97.8% and 96.5%,respectively.The contents of the above-mentioned 4 components in 5 samples from different sources were (1.271±0.045) mg·g^-1,(0.407±0.035) mg·g^-1,(0.906±0.044) mg·g^-1 and (0.325±0.036) mg·g^-1,respectively. Conclusion:The proposed qualitative and quantitative methods provided reference for quality evaluation of roots of Physochlaina phsaloides.