HPLCESIMS法分析山茱萸炮制前后化学成分.docVIP

HPLCESIMS法分析山茱萸炮制前后化学成分 　　 摘 要：目的：建立高效液相色谱-电喷雾-质谱（HPLC-ESI-MS）方法，分析比较山茱萸炮制前后化学成分的变化。方法：采用Agilent Extend-C18色谱柱，乙腈-0.1%甲酸水溶液梯度洗脱；Agilent1200高效液相色谱仪―6410 三重四级杆质谱仪联用；正、负离子检测模式。结果：通过质谱中的主要碎片，在正离子检测模式下，山茱萸生品中检测出了莫诺苷、马钱苷、山茱萸裂苷，制品中检测出了5-羟甲基糠醛、莫诺苷、马钱苷和山茱萸裂苷；在负离子检测模式下，山茱萸生、制品中均检测出了没食子酸、7-O-没食子酰基景天庚酮糖、莫诺苷、山茱萸裂苷。结论：在质谱正、负离子检出模式下，主要化学成分响应均较好，这为分析山茱萸炮制前后化学成分变化，以及控制饮片质量提供了一种新的方法。 　　 关键词：HPLC-ESI-MS；山茱萸；炮制；化学成分 　　中图分类号：R284.1 文献标识码：A 文章编号：1673-7717(2012)01-0062-04 　　Analysis on Active Components in Crude And Processed Cornus Officinals by HPLC-ESI-MS 　　DU Wei?feng1, ZHANG Yun1,CONG Xiao?dong1, CAI Bao?chang1,2 　　(1.Research Center of TCM Processing Technology,Zhejiang Chinese Medical University, Hangzhou 311401,Zhejiang,China; 　　2.Jiangsu Key Laboratory of Chinese Medicine Processing, Nanjing University of Chinese Medicine, Nanjing 210029,Jiangsu,China) 　　Abstract:Objective：To establish an analytical method for comparing the components in crude and processed Cornus officinalis by HPLC-ESI-MS. Methods: These components were analyzed with a Agilent Extend-C18 by gradient elution using 0.1% (V/V) methanoic acid water-solution-acetonitrile as the mobile phase,using Agilent 1200 HPLC-6410 QQQ MS, and detected in positive and negative ion mode. Results: Through fragments mass information in positive ion mode, three compounds(morroniside, lognain and cornuside)were detected in crude drug and four ones(5-HMF, morroniside, lognain and cornuside) in processed product; in negative ion mode, four compounds(gallic acid, 7-O-galloyl-D-sedohep-tulose, morroniside and cornuside) were detected in all crude drug and processed product. Conclusion: In positive and negative ion mode, the main active components all could be detected well. The analytical method could be applied to the intrinsic quality control of crude and processed Cornus officinalis. 　　Key words:HPLC-ESI-MS; Cornus officinalis; processed; active components 　　 　　山茱萸为山茱萸科植物山茱萸Cornus officinalis Sieb. et Zucc.的干燥成熟果肉。临床上多用山萸肉