盐酸麻黄碱有关物质伪麻黄碱检查方法的改进

目的: 针对中国药典2010年版二部盐酸麻黄碱有关物质项下的色谱条件提出修改建议. 方法: 采用Ultimate AQ-C₁₈色谱柱(3.0 mm×250 mm,5 μm),以磷酸盐缓冲溶液(取磷酸二氢钾6.8 g,加三乙胺5 mL,磷酸4 mL,加水至1 000 mL,用稀磷酸或三乙胺调节pH至3.0±0.1)-乙腈(96: 4)为流动相,流速1.0 mL · min^-1,检测波长210 nm,进样量10 μL.在优化后的色谱条件下,麻黄碱峰与伪麻黄碱峰之间的分离度为2.54,麻黄碱峰的理论塔板数为11 232. 结果: 按本文色谱条件及拟定的系统适用性要求对盐酸麻黄碱样品进行有关物质检查,均检测出盐酸伪麻黄碱,使检验结果更加准确可靠. 结论: 本方法经方法学验证,可为提高盐酸麻黄碱质量标准提供参考.

Objective :To put forward modification proposals referring to the Chinese Pharmacopeia 2010 edition of ephedrine hydrochloride chromatographic conditions. Methods :The test was performed on an Ultimate AQ-C₁₈ column(3.0 mm×250 mm,5 μm) with the mobile phase consisted of phosphate buffer solution(potassium dihydrogen take 6.8 g,triethylamine 5 mL,phosphoric 4 mL,add water to 1 000 mL,with dilute phosphoric acid or triethylamine adjusted to pH 3.0±0.1)-acetonitrile(96: 4)at a flow rate of 1.0 mL · min^-1.The detection wavelength was 210 nm,and the injection volume was 10 μL.Under the optimized chromatographic conditions,the separation between ephedrine and pseudoephedrine peaks is 2.54.The theoretical plate number of ephedrine peak is 11 232. Results :According to the established chromatography conditions and the proposed system suitability requirements on material inspection of ephedrine hydrochloride samples,pseudoephedrine hydrochloride was detected at a more accurate and reliable state. Conclusion :The established method has been validated,which can provide a reference for the improvement of quality control of ephedrine hydrochloride.

[1] MIAO YR(苗雨瑞),YANG QH(杨巧荷),YU SY(于姝燕),et al.Research progress of ephedrine and pseudoephedrine(麻黄碱与伪麻黄碱的研究进展)[J].J Inner Mongolia Med Coll(Ade Med Res)(内蒙古医学院学报),2011,33(4):490
[2] YANG WW,DI YY,LI J,et al.Crystal structure and thermodynamic study of ephedrine hydrochloride C₁₀H₁₆NOCl(s)[J].Chem Res Chin Univ,2010,26(2):304
[3] DING HF(丁汉丰),LI SX(李树学),LAN ZM(兰振民),et al.Application of RP-HPLC with pre-column derivatization in the manufacturing process control of synthetic pseudoephedrine hydrochloride(柱前衍生-反相高效液相色谱法在盐酸伪麻黄碱合成中质量控制的应用)[J].Chin J Pharm Anal(药物分析杂志),2009,29(9):1504
[4] ZHU LS(祝莉莎),LIU JK(刘君康),ZHANG JH(张景华),et al.HPLC determination of ephedrine hydrochloride in related substances method research(盐酸麻黄碱中有关物质的HPLC测定方法研究).Chin Pham J(中国药学杂志),2005,40(21):1653
[5] YU CY(于彩岩),WANG H(王海),WANC WQ(王文全),et al.Chinese pharmacopoeia method determination of ephedrine hydrochloride related material and the comparison of foreign pharmacopoeia(中国药典盐酸麻黄碱相关物质测定方法与国外药典的比较)[J].Inner Mongolia Petrochem Ind(内蒙古石油化工),2011(10):22
[6] LIU M(刘敏).Determination of related substances of chloramphenicol and ephedrine nasal drops by HPLC(高效液相色谱法测定氯麻滴鼻液的有关物质)[J].China Pharm(中国药业),2013,22(13):28
[7] LIU XD(刘祥东),LIANG QL(梁琼麟),LUO GA(罗国安),et al.Determination of impurity in ephedrine hydrochloride and pseudoephedrine hydrochloride by HPLC(HPLC法测定盐酸麻黄碱和盐酸伪麻黄碱中杂质)[J].Chin Tradit Herb Drugs(中草药),2005,36(9):40
[8] LI ZW(刘志伟),JIANG TT(蒋婷婷).The determination of ephedrine and its related substances by HPLC method(麻黄碱及其相关物质HPLC的测定方法)[J].J Doctor Visits:2nd Semimonthl y(求医问药:下半月刊),2012,10(9):632
[9] SHI J(师晶),TANG JL(唐景玲),JI HY(纪宏宇),et al.Determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in ephedra water decoction by HPLC(HPLC法测定麻黄水煎液中盐酸麻黄碱和盐酸伪麻黄碱的含量)[J].China Pharm(中国药师),2013,16(2):223
[10] CHENG HJ(成红娟),QU TL(曲婷丽),LIU RL(刘锐玲),et al.Simultaneous determination of ephedrine and pseudoephedrine in Zhisou Lixiao oral liquid by HPLC(HPLC同时测定止嗽立效口服液中盐酸麻黄碱和盐酸伪麻黄碱含量)[J].Chin Tradit Pat Med(中成药),2009,31(2):240
[11] ChP 2010.Vol Ⅱ(中国药典2010年版.二部)[S].2010:777
[12] EP 8.0.2013:2142