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气相色谱-质谱联用法测定大鼠血清中戈米辛A(TJN-101)及其代谢产物

[Determination of gomisin A (TJN-101) and its metabolite in rat serum by gas chromatography-mass spectrometry].

作者信息

Matsuzaki Y, Ishibashi E, Koguchi S, Wakui Y, Takeda S, Aburada M, Oyama T

机构信息

Research Institute for Pharmacology, Tsumura & Co., Ibaraki, Japan.

出版信息

Yakugaku Zasshi. 1991 Oct;111(10):617-20. doi: 10.1248/yakushi1947.111.10_617.

Abstract

Gomisin A (TJN-101) is one of the lignan components isolated from Schisandra Fruits. A high sensitive and precise method for the determination of TJN-101 and its major metabolite (Met. B) in the rat serum was developed by selected ion monitoring (SIM) with gas chromatography-mass spectrometry (GC/MS) using a fused silica capillary column (SPB-1, Supelco). A 100 microliter serum sample was used for the solid phase extraction. The calibration curves of TJN-101 and Met.B both showed a good linearity between 2.0 and 2000.0 ng/ml. The analytical precision (intra-assay, C.V. less than 4.7%), recoveries (98.4 +/- 10.1%), and detection limit (2 ng/ml) of TJN-101 indicated that this system was suited for the determination of TJN-101 in biological fluid. In case of Met.B, the same results as TJN-101, were obtained. After oral administration of TJN-101 at a dose of 10 mg/kg to male rats, the average values of the maximal serum concentration of TJN-101 and Met.B were 1446.1 +/- 131.8 and 317.4 +/- 18.5 ng/ml, respectively. The serum concentrations of these substances could be monitored sufficiently for 8 h after dosing.

摘要

五味子甲素(TJN - 101)是从五味子果实中分离出的木脂素成分之一。采用气相色谱 - 质谱联用仪(GC/MS)的选择离子监测(SIM)模式,使用熔融石英毛细管柱(SPB - 1,Supelco),建立了一种高灵敏度、高精度测定大鼠血清中TJN - 101及其主要代谢产物(代谢物B)的方法。取100微升血清样本进行固相萃取。TJN - 101和代谢物B的校准曲线在2.0至2000.0纳克/毫升之间均呈现良好的线性关系。TJN - 101的分析精密度(批内,变异系数小于4.7%)、回收率(98.4±10.1%)和检测限(2纳克/毫升)表明该系统适用于生物样品中TJN - 101的测定。对于代谢物B,也获得了与TJN - 101相同的结果。雄性大鼠口服剂量为10毫克/千克的TJN - 101后,TJN - 101和代谢物B的最大血清浓度平均值分别为1446.1±131.8和317.4±18.5纳克/毫升。给药后8小时内可充分监测这些物质的血清浓度。

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