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采用液相色谱-串联质谱法同时测定大鼠血浆中紫珠茎和叶中的三种苯乙醇苷及其在药代动力学研究中的应用。

Simultaneous determination of three phenylethanoid glycosides from Callicarpae Caulis et Folium in rat plasma by LC-MS/MS and its application to PK study.

作者信息

Sun Xiuman, Liao Qiongfeng, Liu Guanghui, Cai Hao, Zhang Lei, Zhu Chenchen, Xie Zhiyong

机构信息

School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou 510006, China.

出版信息

Bioanalysis. 2013 Aug;5(15):1883-95. doi: 10.4155/bio.13.124.

DOI:10.4155/bio.13.124
PMID:23905862
Abstract

BACKGROUND

Callicarpae Caulis et Folium (CCF) is a traditional Chinese medicine usually used for hemostasis in clinics. In this study, a novel LC-MS/MS method was developed and validated for the simultaneous quantification of three phenylethanoid glycosides in rat plasma (verbascoside, forsythoside B and poliumoside), which are the major bioactive compounds of CCF; MS was operated in negative mode.

RESULTS

This method was linear between 5.2 and 1010 ng/ml for poliumoside, 7.0 and 420 ng/ml for forsythoside B and 2.60 and 260.0 ng/ml for verbascoside. The MS/MS ion transitions monitored were m/z 769.4→160.5, m/z 755.3→593.3, m/z 623.1→160.5 and m/z 179.0→133.6 for poliumoside, forsythoside B, verbascoside and caffeic acid (IS), respectively. Linearity, accuracy, precision and extraction recovery of three analytes were all satisfactory.

CONCLUSION

The method developed was sensitive, specific and rapid. It has been successfully applied in a PK study of three phenylethanoid glycosides after a single oral administration of CCF extract to rats.

摘要

背景

紫珠茎枝叶是一种常用于临床止血的中药。本研究建立并验证了一种新型液相色谱-串联质谱法,用于同时定量大鼠血浆中的三种苯乙醇苷(毛蕊花糖苷、连翘酯苷B和紫珠苷),这三种成分是紫珠茎枝叶的主要生物活性化合物;质谱采用负离子模式运行。

结果

该方法对紫珠苷的线性范围为5.2至1010 ng/ml,对连翘酯苷B为7.0至420 ng/ml,对毛蕊花糖苷为2.60至260.0 ng/ml。监测的质谱/质谱离子跃迁分别为紫珠苷的m/z 769.4→160.5、连翘酯苷B的m/z 755.3→593.3、毛蕊花糖苷的m/z 623.1→160.5和咖啡酸(内标)的m/z 179.0→133.6。三种分析物的线性、准确度、精密度和提取回收率均令人满意。

结论

所建立的方法灵敏、特异且快速。它已成功应用于大鼠单次口服紫珠茎枝叶提取物后三种苯乙醇苷的药代动力学研究。

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