益母草注射液指纹图谱的研究

目的：建立益母草注射液指纹图谱测定方法。方法：采用高效液相色谱- 蒸发光散射检测法测定益母草注射液指纹图谱。使用阳离子交换色谱柱（4.6 mm×250 mm，5 μm），以甲醇-[0.3% 醋酸铵- 冰醋酸（500:277），pH 2.20]（35:65）为流动相，流速0.8 mL·min^-1，柱温30 ℃，ELSD 漂移管温度80 ℃，载气流速2.0 L·min^-1。并进行方法学验证。结果：本方法重复性、稳定性良好；采用中药指纹图谱相似度评价软件，建立了益母草注射液标准指纹图谱，确定其成分有Cl-、5- 羟甲基-2 糠酸、水苏碱、Na+、K+、胆碱；对31 批样品进行测定，相似度范围为0.957~1.000。结论：方法学验证结果表明，本文建立的HPLC-ELSD 指纹图谱分析法稳定可行，可用于益母草注射液指纹图谱的测定。

Objective:To establish a method for fingerprint analysis of Yimucao injection.Methods:HPLCELSD was used to analyze the fingerprint of Yimucao injection.The conditions were set as follows:Cation exchange chromatography column(4.6 mm×250 mm,5 μm),mobile phase of methanol-［0.3% ammonium acetate-acetic acid(500:277),pH 2.20］(35:65),flow rate at 0.8 mL·min^-1,column temperature at 30 ℃, ELSD drift tube temperature at 80 ℃,flow rate of carrier gas at 2.0 L·min^-1.In addition,the methodology was validated. Results:The repeatability and stability of this method were good.With special software,the standard fingerprint of Yimucao injection was established,including the contents of Cl-,5-hydroxymethyl-2-furoic acid,stachydrine, Na+,K+ and choline.Moreover,31 additional samples were tested and the similarity was from 0.957 to 1.000. Conclusion:The result of methodology validation indicated that the analysis of fingerprint by HPLC-ELSD which is stable and reliable,can be used to analyze the fingerprint of Yimucao injection.

[1] 中国药典2010 年版.一部 [S].2010:272 ChP 2010.Vol Ⅰ[S].2010:272
[2] 申利红, 王胜利.益母草的研究进展[J].安徽农业科学, 2010, 38(8):4414 SHEN LH, WANG SL.Research progress on Leonurus heterophyllus Sweet[J].J Anhui Agric Sci, 2010, 38(8):4414
[3] 汪云伟, 钟恋, 焦小珂, 等.益母草及其制剂的质量控制研究进展[J].中国医药导报, 2014, 11(3):154 WANG YW, ZHONG L, JIAO XK, et al.Research progress on quality control of Leonurus japonicas and its preparations[J].Chin Med Her, 2014, 11(3):154
[4] 何成军, 彭成, 戴鸥, 等.益母草注射液化学成分研究[J].中草药, 2014, 45(21):3048 HE CJ, PENG C, DAI O, et al.Chemical constituents from Leonurus japonicus injection[J].Chin Tradit Herb Drugs, 2014, 45(21): 3048
[5] 何卓琳, 王帅, 孟宪生, 等.基于指纹图谱的益母草胶囊质量控制方法研究[J].中国当代医药, 2013, 20(32):7 HE ZL, WANG S, MENG XS, et al.Study of fingerprint-based quality control method motherwort capsules[J].China Mod Med, 2013, 20(32):7
[6] 贺亚玲, 姜卫东, 何世芬, 等.益母草注射液HPLC 指纹图谱研究[J].药物分析杂志, 2007, 27(10):1578 HE YL, JIANG WD, HE SF, et al.HPLC fingerprint of Yimucao injection[J].Chin J Pharm Anal, 2007, 27(10):1578
[7] 姜卫东, 贺亚玲, 刘仲义.益母草药材与益母草注射液HPLC 特征图谱相关性研究[J].药物分析杂志, 2008, 28(11):1854 JIANG WD, HE YL, LIU ZY.Studies on correlation for HPLC specific chromatogram of Leonurus japonicus Houtt and its injections[J].Chin J Pharm Anal, 2008, 28(11):1854
[8] 陈碧莲, 祝明, 黄卫国, 等.亲水作用色谱- 蒸发光散射法测定益母草中盐酸水苏碱的含量[J].药物分析杂志, 2012, 32(3):502 CHEN BL, ZHU M, HUANG WG, et al.HILIC-ELSD determination of stachydrine hydrochloride in Herba Leonuri[J].Chin J Pharm Anal, 2012, 32(3):502
[9] 李存金, 郭飞宇.HPLC-ELSD 测定复方益母草胶囊中盐酸水苏碱的含量[J].中国现代应用药学, 2013, 30(1):72 LI CJ, GUO FY.Studies on the determination of stachydrine hydrochloride in compound motherwort capsules by HPLC-ELSD[J]. Chin J Mod Appl Pharm, 2013, 30(1):72
[10] 任江剑, 徐建中, 王志安.HPLC 法测定鲜益母草中盐酸水苏碱含量[J].中药新药与临床药理, 2006, 17(3):216 REN JJ, XU JZ, WANG ZA.Determination of stachydrine hydrochloride in fresh medicinal material of Herba Leonuri by HPLC[J].Tradit Chin Drug Res Pharmacol Clin, 2006, 17(3):216
[11] 姜舜尧.益母草药材中水苏碱成分的高效液相色谱法分析[J]. 药物分析杂志, 2001, 21(4):243 JIANG SY.HPLC Analysis of stachydrine in Leonurus japonicus[J]. Chin J Pharm Anal, 2001, 21(4):243
[12] 徐端琼.HPLC-ELSD 测定益母草颗粒中盐酸水苏碱的含量[J]. 中国现代应用药学, 2013, 30(2):189 XU DQ.Determination of stachydrine hydrochloride in Leonuri granule by HPLC-ELSD[J].Chin J Mod Appl Pharm, 2013, 30 (2):189