中国中药杂志

2016, v.41(12) 2235-2244

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UHPLC-LTQ-Orbitrap鉴定苦碟子注射液化学成分及其在大鼠血浆中的移行成分
Rapid characterization of chemical constituents and rats metabolites of Kudiezi injection by UHPLC-LTQ-Orbitrap

刘思燚;张秀平;尚展鹏;王菲;张晓昕;张加余;卢建秋;
LIU Si-yi;ZHANG Xiu-ping;SHANG Zhan-peng;WANG Fei;ZHANG Xiao-xin;ZHANG Jia-yu;LU Jian-qiu;School of Chinese Pharmacy,Beijing University of Chinese Medicine;Beijing Institution of Chinese Medicine,Beijing University of Chinese Medicine;Library of Beijing University of Chinese Medicine;

摘要(Abstract):

应用UHPLC-HR-MSn技术分析检测苦碟子注射液中原型成分及其在大鼠体内的代谢物。尾静脉注射苦碟子注射液后,收集给药前后的大鼠血浆,经固相萃取进行处理后,采用ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱和0.1%甲酸水溶液(A)-乙腈(B)流动相系统进行梯度洗脱。应用LTQ-Orbitrap质谱负离子模式检测苦碟子注射液中的化学成分以及血浆样品中的原型成分和代谢产物。根据精确相对分子质量数据和多级质谱碎片,结合对照品比对,从苦碟子注射液中分析鉴定了53个成分,包括18个有机酸、15个黄酮、18个倍半萜内酯、2个核苷;从大鼠血浆中分析检测了38个原型及代谢产物,主要代谢途径为甲基化、羟基化、水解、葡萄糖酸酸化及它们的复合反应等。应用UHPLC-LTQ-Orbitrap高分辨液质联用技术较为全面地阐明了苦碟子注射液化学成分及其在大鼠血浆中的移行成分,为进一步研究苦碟子注射液体内代谢过程以及药效物质基础提供了科学依据。
A rapid and sensitive UHPLC-HR-MSnmethod was used for the identification of Kudiezi injection and its main metabolites in rat plasma. After the tail intravenous injection of Kudiezi,ACQUITY UHPLC BEH C_(18)( 2. 1 mm × 100 mm,1. 7 μm) was used,with 0. 1% formic acid-acetonitrile solution as the mobile phase for gradient elution. Kudiezi injection and plasma were detected by ESI-LTQ-Orbitrap equipped with an ESI ion source in a negative mode. Based on the accurate mass measurements,the retention time and the mass fragmentation patterns,a total of 53 compounds were tentatively identified and characterized. Furthermore,metabolites in rat plasma after the intravenous administration of Kudiezi injection were also analyzed. A total of 38 compounds were identified,including 27 prototypes and 11 metabolites through metabolic pathways of methylation,glucuronide conjugation,sulfate conjugation and hydrolysis. As a result,UHPLC-LTQ-Orbitrap technique was applied to comprehensively expound Kudiezi injection's chemical components and constituents migrating to rat plasma,and provide scientific basis for further studies on Kudiezi injection' s in vivo metabolic process and effective material base.

关键词(KeyWords): 苦碟子注射液;液质联用技术;化学成分;代谢产物鉴定
Kudiezi injection;UHPLC-LTQ-Orbitrap;chemical constituents;metabolites identification

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基金项目(Foundation): 国家重点基础研究发展计划(973)项目(2012CB518406);; 北京中医药大学自主选题项目(2016-JYB-XS075)

作者(Author): 刘思燚;张秀平;尚展鹏;王菲;张晓昕;张加余;卢建秋;
LIU Si-yi;ZHANG Xiu-ping;SHANG Zhan-peng;WANG Fei;ZHANG Xiao-xin;ZHANG Jia-yu;LU Jian-qiu;School of Chinese Pharmacy,Beijing University of Chinese Medicine;Beijing Institution of Chinese Medicine,Beijing University of Chinese Medicine;Library of Beijing University of Chinese Medicine;

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