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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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HPLC-Q-Orbitrap-MS法分析大鼠血浆中六神丸醇提物的入血成分及其代谢产物

Study on absorbed prototype components and metabolites of ethanolic extracts from Liushen pills in rat plasma by HPLC-Q-Orbitrap-MS

分类号:R917
出版年·卷·期(页码):2020,40 (4):633-643
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的: 应用高效液相色谱-静电场轨道阱高分辨质谱(HPLC-Q-Orbitrap-MS)技术对六神丸醇提物在大鼠血浆中的入血极性成分及其代谢产物进行分析。方法: 采用乙腈沉淀蛋白法进行样品前处理,在C18色谱柱(4.6 mm×250 mm,5 μm)上,以乙腈-0.2%甲酸水溶液为流动相梯度洗脱,在电喷雾正负离子同时采集的模式下分别获得六神丸乙醇提取物、空白血浆和含药血浆样品的液相色谱-质谱信息。结果: 通过质谱数据、对照品比对,初步鉴定了9个原型入血成分和19个代谢产物,其中蟾蜍二烯内酯类成分以去乙酰化、羟基化和异构化代谢产物为主,胆酸类成分以与甘氨酸结合产物为主,同时存在脱氧和羟基化产物。另发现血浆中的6种氨基酸在给药后含量显著增加。结论: 本研究建立的HPLC-Q-Orbitrap-MS分析方法能有效地鉴别六神丸醇提物在体内的极性代谢成分群,为六神丸醇提取物的抗肝癌药效物质及其作用机制研究提供科学依据。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To examine the absorbed prototype components and metabolites of ethanolic extracts from Liushen pills in rat plasma by HPLC-Q-Orbitrap-MS. Methods: The plasma samples were pre-treated with acetonitrile to precipitate proteins. LC separation was performed on a C18 column(4.6 mm×250 mm,5 μm),with 0.2% formic acid aqueous solution and acetonitrile as mobile phase in a gradient elution mode. LC-MS information of blank plasma and plasma samples were collected in both positive and negative ions modes. Results: 9 Prototype components and 19 metabolites in the rat plasma were initially identified. Among them,bufadienolides were mainly metabolized by deacetylation,hydroxylation and isomerization,while metabolites of bile acids were mainly composed of binding products with glycine,and there was a dynamic balance of deoxidation and hydroxylation. In addition,6 amino acids were found to increase significantly after drug administration. Conclusion: This study undertakes comprehensive and accurate identification of the metabolites of polar components from Liushen pills,which provides scientific evidences for research on the components and mechanism of anti-liver tumor function of Liushen pills.

-----参考文献:---------------------------------------------------------------------------------------
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