HPLC-可变双波长法测定麻黄不同炮制品中麻黄类生物碱和川芎嗪的含量  

Determination of ephedrine alkaloids and 2,3,5,6-tetramethyl pyrazine in ephedra herba and its processed products by variable dual wavelength HPLC

作　　者：钱琨[1] 张克霞[1] 刘子莹[2] 赵思敏[2] 毕开顺[2] 陈晓辉[2] 

机构地区：[1]沈阳药科大学中药学院,辽宁沈阳110016 [2]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2015年第7期531-536,共6页Journal of Shenyang Pharmaceutical University

基　　金：国家自然科学基金资助项目(81373367)

摘　　要：目的建立同时测定麻黄及其不同炮制品中盐酸麻黄碱（1）,盐酸伪麻黄碱（2）,盐酸甲基麻黄碱（3）和川芎嗪（4）含量的方法。方法采用HPLC法,Agilent TC-C18柱（250 mm×4.6 mm,5μm）,流动相：乙腈-水-磷酸-三乙胺（体积比为4.0∶96.0∶0.1∶0.1）,流速：0.8 m L·min-1,柱温：30℃,检测波长：（0～22 min）210、（22～30 min）300 nm。结果化合物1-4分别在18.30～366.1、17.87～357.4、5.070～101.4、0.3050～6.100 mg·L-1质量浓度内,峰面积线性关系良好（r≥0.999 6）,平均加样回收率分别为98.7%（RSD=1.8%）、100.9%（RSD=1.6%）、100.8%（RSD=1.6%）和97.7%（RSD=1.3%）。该方法应用于麻黄及其不同炮制品中麻黄类生物碱和川芎嗪的含量测定,测得化合物1-4的含量质量分数分别为0.83%～1.0%、0.48%～0.84%、0.087%～0.22%和0.001 7%～0.009 0%。结论麻黄经炮制后,4种化合物含量均发生了不同程度的改变,表明炮制方法对麻黄化学成分的含量影响较大,该分析方法的建立为控制不同炮制品的质量提供了一定的参考依据。Objective To establish an HPLC method for simultaneous determination of ephedrine hydrochloride（ 1）,pseudoephedrine hydrochloride（ 2）,methylephedrine hydrochloride（ 3） and 2,3,5,6-tetramethyl pyrazine（ 4） in the products of Ephedra sinica Stapf processed by different methods. Methods The chromatographic separation was performed on an Agilent TC-C18column（ 4. 6 mm × 250 mm,5 μm） with mobile phase of acetonitrile-water-phosphoric acid-triethylamine（ V ∶ V ∶ V ∶ V = 4. 0 ∶ 96. 0 ∶ 0. 1 ∶ 0. 1） at a flowrate of0. 8 m L·min- 1. The column temperature was set at 30 ℃ and the detection wavelength was set at 210 nm in0- 22 min and 300 nm in 22- 30 min. Results The standard curves of compounds 1- 4 showed good linearity（ r≥0. 999 6） in the ranges of 18. 30- 366. 1,17. 87- 357. 4,5. 070- 101. 4,0. 305 0- 6. 100 mg·L- 1with the corresponding average recoveries of 98. 7%（ RSD = 1. 8%）,100. 9%（ RSD = 1. 6%）,100. 8%（ RSD = 1. 6%） and 97. 7%（ RSD = 1. 3%）（ n = 6）,respectively. The contents determination of 1- 4 were0. 83%- 1. 0%,0. 48%- 0. 84%,0. 087%- 0. 22% and 0. 001 7%- 0. 009 0%,respectively. Conclusions To some extent,the contents of the major components vary in different processed products of Ephedra sinica Stapf. The results indicate that different processing methods cause significant differences in the contents of the major components of Ephedra sinica Stapf. It is of great use for further researching the relevance of the processing methods to pharmacodynamics of Ephedra sinica Stapf.

关 键 词：高效液相色谱法 盐酸麻黄碱 盐酸伪麻黄碱 盐酸甲基麻黄碱 川芎嗪 炮制品 

分 类 号：R28[医药卫生—中药学]