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超高效液相色谱-质谱联用同时分析十二种胆汁酸及探讨发酵法炮制天南星的作用机制

Simultaneous Analysis of Twelve Bile Acids by UPLC-MS and Exploration of the Processing Mechanism of Bile Arisaema by Fermentation.

作者信息

Zhao Qimiao, Shan Guoshun, Xu Dan, Gao Hui, Shi Ji, Ju Chengguo, Lin Guimei, Zhang Fan, Jia Tianzhu

机构信息

School of Pharmacy, Liaoning University of Traditional Chinese Medicine, Dalian, China.

出版信息

J Anal Methods Chem. 2019 Sep 9;2019:2980596. doi: 10.1155/2019/2980596. eCollection 2019.

Abstract

Ultrahigh-performance liquid chromatography (UPLC) coupled with quadrupole time-of-flight tandem mass spectrometry (Q/TOF-MS) in the MS/MS mode and UPLC coupled with triple quadrupole mass spectrometry (QqQ-MS) using the multiple reaction monitoring (MRM) mode were used to make a qualitative and quantitative analysis of twelve bile acids in Bile Arisaema. The fragmentation pathway of twelve bile acids was proposed. The quantification method showed a good linearity over a wide concentration range (  > 0.99), repeatability (RSD < 4.12%), stability (RSD < 4.25%), precision (RSD < 4.06%), and recovery (95.36-102.15%). Content of twelve compounds in Bile Arisaema varied significantly depending on region. Chemometric methods, hierarchical clustering analysis (HCA), and principal components analysis (PCA) were successfully used to optimize the fermentation time of the Bile Arisaema. The results suggested that the Bile Arisaema could complete fermentation in 15 days. The possible processing mechanism of Bile Arisaema promoted the transformation of conjugated bile acids into free bile acids in fermentation.

摘要

采用超高效液相色谱(UPLC)与处于串联质谱模式(MS/MS)的四极杆飞行时间串联质谱(Q/TOF-MS)联用,以及采用多反应监测(MRM)模式的UPLC与三重四极杆质谱(QqQ-MS)联用,对胆南星中的12种胆汁酸进行定性和定量分析。提出了12种胆汁酸的裂解途径。该定量方法在较宽的浓度范围内显示出良好的线性(>0.99)、重复性(RSD<4.12%)、稳定性(RSD<4.25%)、精密度(RSD<4.06%)和回收率(95.36 - 102.15%)。胆南星中12种化合物的含量因产地不同而有显著差异。化学计量学方法,即层次聚类分析(HCA)和主成分分析(PCA),成功用于优化胆南星的发酵时间。结果表明,胆南星可在15天内完成发酵。胆南星可能的炮制机制促进了发酵过程中共轭胆汁酸向游离胆汁酸的转化。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/755d/6754901/f7723a606fe9/JAMC2019-2980596.001.jpg

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