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超高效液相色谱-串联质谱法测定大鼠口服防己黄芪汤和粉防己提取物后血浆中的粉防己碱和防己诺林碱。

Ultra high performance liquid chromatography with tandem mass spectrometry method for the determination of tetrandrine and fangchinoline in rat plasma after oral administration of Fangji Huangqi Tang and Stephania tetrandra S. Moore extracts.

作者信息

Wang Xiaoli, Liu Xiao, Cai Hao, Pei Ke, Cao Gang, Xu Xiaoyan, Shi Fa, Cai Baochang

机构信息

College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, P. R. China; Nanjing Haichang Chinese Medicine Group Corporation, Nanjing, P. R. China.

出版信息

J Sep Sci. 2015 May;38(8):1286-93. doi: 10.1002/jssc.201401384. Epub 2015 Mar 10.

Abstract

A rapid, sensitive, and reliable analytical method based on ultra high performance liquid chromatography with tandem mass spectrometry has been developed for the simultaneous determination of fangchinoline and tetrandrine in rat plasma. Plasma samples were pretreated by protein precipitation with acetonitrile. The analysis was performed on a C18 reversed-phase ultra high performance liquid chromatography column (2.1 mm × 100 mm, 3.5 μm, Agilent), and the flow rate was set at 0.4 mL/min. Under the experimental conditions, extraction recoveries from plasma were 68.1-72.8% for fangchinoline and 69.2-76.5% for tetrandrine. The plasma concentrations of tetrandrine and fangchinoline in rats at assigned time points were all successfully detected through exactly validated method. Good linearities were obtained in the range of 0.92-184 ng/mL for tetrandrine and in the range of 0.83-166 ng/mL for fangchinoline. The intra- and interday precisions for both analytes were within 11.1% and the accuracies were within the range of -10.7 to 11.3%. The developed method was then successfully applied to investigate the pharmacokinetic properties of these two alkaloids after oral administration of Stephania tetrandra S. Moore extracts and Fangji Huangqi Tang. The comparative results provided a meaningful basis for a better understanding of the practical value of the compatibility theory of traditional Chinese medicine in the clinic.

摘要

已开发出一种基于超高效液相色谱-串联质谱的快速、灵敏且可靠的分析方法,用于同时测定大鼠血浆中的粉防己碱和防己诺林碱。血浆样品通过乙腈沉淀蛋白进行预处理。分析在C18反相超高效液相色谱柱(2.1 mm×100 mm,3.5μm,安捷伦)上进行,流速设定为0.4 mL/min。在实验条件下,粉防己碱的血浆提取回收率为68.1 - 72.8%,防己诺林碱为69.2 - 76.5%。通过经过准确验证的方法成功检测出大鼠在指定时间点的血浆中防己诺林碱和粉防己碱的浓度。防己诺林碱在0.92 - 184 ng/mL范围内、粉防己碱在0.83 - 166 ng/mL范围内均获得良好的线性关系。两种分析物的日内和日间精密度均在11.1%以内,准确度在 - 10.7%至11.3%范围内。然后将所开发的方法成功应用于研究口服粉防己提取物和防己黄芪汤后这两种生物碱的药代动力学性质。比较结果为更好地理解中药配伍理论在临床中的实际价值提供了有意义的依据。

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