摘要
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,5μm),以乙腈-醋酸钠缓冲液(p H 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、20~100μg·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（p H 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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第1期175-180,共6页
Chinese Journal of Pharmaceutical Analysis
基金
"杀粘"蒙药泡囊草化学成分
质量标准及抗菌作用研究(内蒙古自治区研究生科研创新资助项目)
项目编号S20161013602
内蒙古自治区蒙医药科技重大专项子课题(GCY201508020)
