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[摘要]
目的 建立基于UPLC-DAD-TOF/MS结合HPLC-UV法检测麻黄样品化学成分的方法,以明确麻黄"先煎去沫"样品化学成分间的差异。方法 UPLC-DAD-TOF/MS:Waters ACQUITY UPLC® BEH C18(50 mm×2.1 mm,1.7μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相梯度洗脱,体积流量0.3 mL/min,柱温40℃,正、负离子模式扫描;HPLC-UV:以十八烷基硅烷键合硅胶为填充剂(150 mm×4.6 mm,5μm),以0.1%磷酸水溶液(含0.05%三乙胺)-乙腈溶液(99:1)为流动相,等度洗脱,体积流量1 mL/min,检测波长为210 nm,柱温30℃。结果 上沫中所含成分较少,去沫下液和全煎煮液中化学成分基本一致。同时,三者均可鉴定出去甲基麻黄碱、去甲基伪麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱5个生物碱类成分和1个羧酸类成分(4-羟基-7-甲氧基-2-喹啉羧酸)。但上沫中生物碱含量极低,而全煎煮液中3种生物碱的含量略高于去沫下液。结论 麻黄"先煎去"沫理论可能与生物碱类成分关系不大,但仍需后期进行更深入的研究验证。
[Key word]
[Abstract]
Objective To establish a method for detecting the chemical compositions of "decocted first and defoamed" of Ephedra Herba by UPLC-DAD-TOF/MS coupled with HPLC-UV, so as to clarify the difference of chemical constituents among them. Methods The analysis was performed on an ACQUITY UPLC® BEH C18 column (50 mm×2.1 mm, 1.7 μm) by UPLC-DAD-TOF/MS with gradient elution. The mobile phase consists of methanol and 0.1% formic acid-water at a flow rate of 0.3 mL/min. The column temperature was 40℃. The information of compounds was acquired on positive and negative mode. Similarly, HPLC-UV was applied for measuring the content of alkaloids respectively. The C18 column was used, the mobile phase was acetonitrile-0.1% phosphoric acid (containing 0.05% triethylamine) (99:1) at the flow rate of 1 mL/min, the detective wavelength was set up at 210 nm, and the column temperature was 30℃. Results There were less content in the upper foam, and the chemical components in the lower liquid and the whole liquid were basically same. Five alkaloids and one carboxylic acid (4-hydroxy-7-methoxyl-2-quinoline carboxylic acid) was identified from all kinds of liquids. However, the content of alkaloids in the upper foam was very low, and the content of three alkaloids in the whole solution was slightly higher than that in the lower liquid. Conclusion The defoamed method may not be related to the chemical compositions of alkaloids, but it still needs further research and verification.
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[基金项目]
天津市中医药管理局天津市卫生和计划生育委员会中西医结合科研课题(2015142)