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摘要：目的 建立毛细管电泳分离麻黄碱与伪麻黄碱的方法。方法 分别以甲基化-β-环糊精和羟丙基-β-环糊精为添加剂，采用毛细管电泳法分离麻黄碱和伪麻黄碱。考察添加剂的种类和浓度、缓冲溶液的浓度和pH值、运行电压、有机溶剂对麻黄碱和伪麻黄碱分离的影响。结果 采用甲基化-β-环糊精和羟丙基-β-环糊精为添加剂均可以使麻黄碱和伪麻黄碱实现分离。前者的最佳分离条件为：分离电压10 kV，25 mmol/L Tris-磷酸缓冲液（pH 2.42）含20 mg/mL甲基化-β-环糊精，此条件下麻黄碱和伪麻黄碱的分离度为1.56，在13 min内获得快速基线分离；后者的最佳分离条件为：分离电压10 kV，25 mmol/L Tris-H3PO4缓冲液（pH 3.00）含50 mg/mL羟丙基-β-环糊精，此条件下麻黄碱和伪麻黄碱的分离度为2.73，在15 min内获得快速基线分离。结论 此方法可靠、快速、重复性好，可作为麻黄碱和伪麻黄碱分离测定的方法。
关键词：麻黄碱；伪麻黄碱；毛细管电泳；环糊精
DOI：10.3969/j.issn.1005-5304.2016.11.022
中图分类号：R284.2 文献标识码：A 文章编号：1005-5304（2016）11-0090-04
Abstract： Objective To establish a capillary electrophoresis method to separate ephedrine and psedudoephedrine. Methods RM-β-CD and HP-β-CD were set as additives. A capillary electrophoresis method was set up. The effects of types and concentrations of additives， the concentrations and pH values of buffered solution， running voltage and organic solvent on the separation of ephedrine and psedudoephedrine were investigated. Results Ephedrine and pseudoephedrine could be successfully separated by using either RM-β-CD or HP-β-CD as additives. When RM-β-CD was used as additive， the best separation conditions were as follows： separation voltage 10 kV， 25 mmol/L Tris-H3PO4 （pH 2.42）， 20 mg/mL of RM-β-CD. Under the conditions， the resolution of ephedrine and pseudoephedrine was 1.56 and they were separated successfully within 13 min. When HP-β-CD was used as additive， the best separation conditions were as follows： separation voltage 10 kV， 25 mmol/L Tris-H3PO4 （pH 3.00）， 50 mg/mL of HP-β-CD. Under the conditions， the resolution of ephedrine and pseudoephedrine was 2.73 and they were separated successfully within 15 min. Conclusion This method is reliable， rapid and repeatable. It can be used as separation determination method for ephedrine and pseudoephedrine.
Key words： ephedrine； pseudoephedrine； capillary electrophoresis； cyclodextrin
麻黃具有发汗解表、宣肺平喘等功效，生物碱类成分是其主要活性成分，其中麻黄碱和伪麻黄碱是最主要的活性成分，二者互为立体异构体。麻黄碱具有平喘、抑制高血糖、兴奋中枢神经和交感神经等作用，伪麻黄碱具有抗炎和利尿作用，是麻黄药材质量控制的指标性成分[1]。目前分离麻黄碱和伪麻黄碱的方法主要有高效液相色谱法[2-4]、气相色谱法[5-6]、薄层扫描法[7]、毛细管电泳法[8-10]等。毛细管电泳法由于分离速度快、模式多、消耗少等特点在手性分离分析中具有明显优势。目前采用毛细管电泳法对麻黄碱和伪麻黄碱进行分离的报道，主要是在分离过程中加入氨基酸[11]、络合物[12-13]、离子液体[14]、有机添加剂[15]等改变二者的淌度，或对二者进行衍生后改变淌度使其分离[16]。本试验以环糊精衍生物为添加剂，采用毛细管电泳分离麻黄碱与伪麻黄碱，为麻黄的质量控制提供新思路。
1 仪器与试药
毛细管规格为75 mm内径，360 mm外径（河北永年锐沣色谱器件有限公司）。TriSep-2100电色谱系统（通微，Unimicro Technologies），TriSep2003色谱工作站（通微，Unimicro Technologies），FE20/EL20实验室pH计，梅特勒-托利多仪器（上海）有限公司。
关键词：麻黄碱；伪麻黄碱；毛细管电泳；环糊精
DOI：10.3969/j.issn.1005-5304.2016.11.022
中图分类号：R284.2 文献标识码：A 文章编号：1005-5304（2016）11-0090-04
Abstract： Objective To establish a capillary electrophoresis method to separate ephedrine and psedudoephedrine. Methods RM-β-CD and HP-β-CD were set as additives. A capillary electrophoresis method was set up. The effects of types and concentrations of additives， the concentrations and pH values of buffered solution， running voltage and organic solvent on the separation of ephedrine and psedudoephedrine were investigated. Results Ephedrine and pseudoephedrine could be successfully separated by using either RM-β-CD or HP-β-CD as additives. When RM-β-CD was used as additive， the best separation conditions were as follows： separation voltage 10 kV， 25 mmol/L Tris-H3PO4 （pH 2.42）， 20 mg/mL of RM-β-CD. Under the conditions， the resolution of ephedrine and pseudoephedrine was 1.56 and they were separated successfully within 13 min. When HP-β-CD was used as additive， the best separation conditions were as follows： separation voltage 10 kV， 25 mmol/L Tris-H3PO4 （pH 3.00）， 50 mg/mL of HP-β-CD. Under the conditions， the resolution of ephedrine and pseudoephedrine was 2.73 and they were separated successfully within 15 min. Conclusion This method is reliable， rapid and repeatable. It can be used as separation determination method for ephedrine and pseudoephedrine.
Key words： ephedrine； pseudoephedrine； capillary electrophoresis； cyclodextrin
麻黃具有发汗解表、宣肺平喘等功效，生物碱类成分是其主要活性成分，其中麻黄碱和伪麻黄碱是最主要的活性成分，二者互为立体异构体。麻黄碱具有平喘、抑制高血糖、兴奋中枢神经和交感神经等作用，伪麻黄碱具有抗炎和利尿作用，是麻黄药材质量控制的指标性成分[1]。目前分离麻黄碱和伪麻黄碱的方法主要有高效液相色谱法[2-4]、气相色谱法[5-6]、薄层扫描法[7]、毛细管电泳法[8-10]等。毛细管电泳法由于分离速度快、模式多、消耗少等特点在手性分离分析中具有明显优势。目前采用毛细管电泳法对麻黄碱和伪麻黄碱进行分离的报道，主要是在分离过程中加入氨基酸[11]、络合物[12-13]、离子液体[14]、有机添加剂[15]等改变二者的淌度，或对二者进行衍生后改变淌度使其分离[16]。本试验以环糊精衍生物为添加剂，采用毛细管电泳分离麻黄碱与伪麻黄碱，为麻黄的质量控制提供新思路。
1 仪器与试药
毛细管规格为75 mm内径，360 mm外径（河北永年锐沣色谱器件有限公司）。TriSep-2100电色谱系统（通微，Unimicro Technologies），TriSep2003色谱工作站（通微，Unimicro Technologies），FE20/EL20实验室pH计，梅特勒-托利多仪器（上海）有限公司。