杨立新;冯伟红;夏伯候;林丽美;刘薇薇;苗婉清;甘国锋;邹济高;李春;
YANG Li-xin;FENG Wei-hong;XIA Bo-hou;LIN Li-mei;LIU Wei-wei;MIAO Wan-qing;GAN Guo-feng;ZOU Ji-gao;LI Chun;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines;Hunan University of Chinese Medicine;Wuxi Jiminkexin Shanhe Pharmaceutical Co.,Ltd.;Qingxu County People's Hospital of Shanxi Province;

• 1:中国中医科学院中药研究所
• 2:中药质量控制技术国家工程实验室
• 3:湖南中医药大学
• 4:无锡济民可信山禾药业股份有限公司

摘要(Abstract)：

该研究采用高效液相色谱法建立并分析了不同厂家生产醒脑静注射液的特征图谱。采用Thermo BDS Hypersil C18色谱柱(4.6 mm×250 mm,5μm)进行分离,流动相为乙腈-0.02%甲酸水溶液,梯度洗脱,流速1.0 m L·min~(-1),检测波长254nm,柱温35℃,进样量20μL。通过对29批醒脑静注射液的HPLC特征图谱研究,共标定了11个特征峰。经与对照品对比,指认出其中7个特征峰的结构,分别为优香芹酮、樟脑、姜黄烯酮、莪术烯醇、莪术二酮、莪术酮和吉马酮。运用计算机辅助相似性评价系统及主成分分析对所建29批醒脑静注射液的HPLC特征图谱进行分析比较,结果显示不同厂家生产的醒脑静注射液能明显分为3类。该文所建立的HPLC特征图谱为科学评价和有效控制醒脑静注射液质量提供了依据。
To establish and analyze the HPLC specific chromatograms of Xingnaojing injection manufactured by different factories.The separation was performed on a Thermo BDS Hypersil C_(18)column( 4. 6 mm × 250 mm,5 μm),with the mobile phase consisting of acetonitrile-0. 02% formic acid aqueous solution for gradient elution. The flow rate was 1. 0 m L·min~(-1),and the column temperature was 35 ℃. The detection wavelength was set at 254 nm,and the sample size was 20 μL. Eleven chromatographic peaks were identified as characteristic peaks of HPLC specific chromatograms of Xingnaojing injection,after analyzing 29 batches of Xingnaojing injection samples. Compared with the reference substances,seven of them were identified as eucarvone,camphor,curcumenone,curcumenol,curdione,curzerenone and germacrone,respectively. HPLC specific chromatograms of Xingnaojing injection manufactured by three factories could be easily classified into three categories after investigation with computer-aided similarity evaluation system combined with principal component analysis. The established HPLC specific chromatograms provide a basis for scientific evaluation and effective con-trol of the quality of Xingnaojing injection.

关键词(KeyWords)： 醒脑静注射液;特征图谱;主成分分析;高效液相色谱法
Xingnaojing injection;specific chromatograms;principal component analysis(PCA);high-performance liquid chro matography(HPLC)

Abstract:

Keywords:

基金项目(Foundation): 北京市自然科学基金项目(7132152);; 中央级公益性科研院所基本科研业务费专项(ZZ070828)

作者(Author): 杨立新;冯伟红;夏伯候;林丽美;刘薇薇;苗婉清;甘国锋;邹济高;李春;
YANG Li-xin;FENG Wei-hong;XIA Bo-hou;LIN Li-mei;LIU Wei-wei;MIAO Wan-qing;GAN Guo-feng;ZOU Ji-gao;LI Chun;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines;Hunan University of Chinese Medicine;Wuxi Jiminkexin Shanhe Pharmaceutical Co.,Ltd.;Qingxu County People's Hospital of Shanxi Province;

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DOI:

参考文献(References)：

• [1]聂黎行,石上梅,翟为民,等.指纹图谱技术在中药注射液标准提高中的应用[J].中成药,2015,37(3):607.
• [2]中国药典.一部[S].2015:1529,1108.
• [3]Peng W,Yang J,Wang Y,et al.Systematic review and Metaanalysis of randomized controlled trials of Xingnaojing treatment for stroke[J].Evid Based Complement Alternat Med,2014,doi:10.1155/2014/210851.
• [4]国家食品药品监督管理局.国家药品标准WS3-B-3353-98-2003[S].2003.
• [5]魏宁漪,马长华,段天璇.固相微萃取-气相色谱法测定醒脑静注射剂中的麝香酮[J].色谱,2005,23(5):565.
• [6]吴建伟,魏晓舒.醒脑静注射液中麝香酮的含量测定[J].中草药,1999,30(4):272.
• [7]吴小英.毛细管气相色谱法测定醒脑静葡萄糖注射液中冰片和麝香酮含量[J].安徽医药,2008,12(2):129.
• [8]高文分,袁文娟,王梅.GC法同时测定醒脑静注射液中麝香酮、龙脑的含量及有关物质[J].中国药师,2011,14(11):1607.
• [9]赵希贤,方颖,赵鸣舒,等.醒脑静注射液质量分析[J].中国实验方剂学杂志,2011,17(22):75.
• [10]方颖,赵希贤,赵鸣舒,等.气相色谱法同时测定醒脑静注射液中麝香酮、龙脑、樟脑、异龙脑的含量[J].中国实验方剂学杂志,2012,18(8):96.
• [11]高文分,袁文娟,王梅.气相色谱法拆分醒脑静注射液中龙脑对映体及含量测定[J].药物分析杂志,2012,32(5):873.
• [12]张琼丹,刘东辉,林微微,等.手性气相色谱法分析醒脑静注射液[J].中药新药与临床药理,2012,23(3):338.
• [13]陈琴华,李鹏,张卓.GC-MS-SIM法测定醒脑静注射液中麝香酮的含量[J].中国医院药学杂志,2009,29(5):422.
• [14]王立强,王思玲,苏德森.醒脑静注射液质量控制研究[J].中成药,2004,26(4):289.
• [15]尹国平,张清哲,安月伟,等.温郁金化学成分及药理活性研究进展[J].中国中药杂志,2012,37(22):3354.
• [16]王秀.莪术二酮抗血栓和抗血小板聚集作用研究[D].合肥:安徽医科大学,2012.
• [17]孟祥乐,李红伟,李颜,等.栀子化学成分及其药理作用研究进展[J].中国新药杂志,2011,20(11):959.