中国中药杂志

2017, v.42(09) 1685-1692

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三黄片化学成分的UPLC-Q-TOF-MS/MS快速鉴定分析
UPLC-Q-TOF/MS for rapid analysis of chemical constituents in Sanhuang tablets

刘梦娇;王云;李玲云;李晓庆;戴业佳;张雪;麻印莲;张村;李文兰;
LIU Meng-jiao;WANG Yun;LI Ling-yun;LI Xiao-qing;DAI Ye-jia;ZHANG Xue;MA Yin-lian;ZHANG Cun;LI Wen-lan;Research Center on Life Sciences and Environmental Sciences,Harbin University of Commerce;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;School of Pharmacy,Henan University of Chinese Medicine;School of Pharmacy,Anhui University of Chinese Medicine;

摘要(Abstract):

建立复方三黄片中化学成分的超高效液相色谱串联四极杆飞行时间质谱(UPLC-Q-TOF-MS/MS)定性分析方法,选用Waters ACQUITY BEH C_(18)超高效液相色谱柱(2.1 mm×100 mm,1.7μm),采用梯度洗脱,以0.1%甲酸水(A)-0.1%甲酸乙腈(B)为流动相,流速0.2 m L·min~(-1),进样量1μL,柱温为30℃;电喷雾离子源(Waters-Xevo G2 Q-TOF),干燥气温度325℃,以四极杆飞行时间质谱为检测器进行检测。结合文献报道和质谱数据,通过串联质谱对复方三黄片中的化学成分进行了结构鉴定,共鉴定了38个化合物,包括1个生物碱类成分,1个二蒽酮类化合物,6个鞣质类成分,7个蒽醌苷类成分,6个游离蒽醌类成分,17个黄酮类成分。采用液质联用技术鉴定复方三黄片中的化学成分,快速简便,结果可靠,有助于揭示复方三黄片的化学成分及其药效物质。
The qualitative analysis method of ultra performance liquid chromatography tandem quadrupole time of flight mass spectrometry( UPLC-Q-TOF-MS/MS) was established for the chemical constituents in Sanhuang tablets. Waters ACQUITY BEH C_(18)(2. 1mm × 100 mm,1. 7 μm) column was used with 0. 1% formic acid solution( A)-0. 1% formic acid acetonitrile( B) as the mobile phase for gradient elution. The flow rate was 0. 2 m L·min~(-1); the sample volume was 1 μL and the column temperature was 30 ℃.The high-resolution quadrupole time-flight mass spectrometry was used as detector with electrospray ion source in both positive and negative models,and the dry gas temperature was 325 ℃. Based on the analysis of mass spectrometry and literature reports,38 compounds were confirmed,including 1 alkaloid,1 dianthrone compound,6 tannins,7 anthraquinone glycosides,6 anthraquinones and 17 flavonoids. Liquid chromatography-mass spectrometry method is simple,reliable and rapid to identify the chemical compositions of Sanhuang tablets,and it is helpful to reveal its chemical constituents and pharmacodynamic substances.

关键词(KeyWords): 三黄片;大黄;黄芩;小檗碱;液质联用
Sanhuang tablets;rhubarb;baicalin;berberine;HPLC-MS

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基金项目(Foundation): 国家“重大新药创制”科技重大专项(2014ZX09304307001)

作者(Author): 刘梦娇;王云;李玲云;李晓庆;戴业佳;张雪;麻印莲;张村;李文兰;
LIU Meng-jiao;WANG Yun;LI Ling-yun;LI Xiao-qing;DAI Ye-jia;ZHANG Xue;MA Yin-lian;ZHANG Cun;LI Wen-lan;Research Center on Life Sciences and Environmental Sciences,Harbin University of Commerce;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;School of Pharmacy,Henan University of Chinese Medicine;School of Pharmacy,Anhui University of Chinese Medicine;

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