Feng Duiping, Qiu Feng, Tong Zhanqi, Xie Chunming
Department of Interventional Radiology, First Hospital of Shanxi Medical University, Taiyuan, 030001, China.
J Chromatogr Sci. 2013 Apr;51(4):335-40. doi: 10.1093/chromsci/bms145. Epub 2012 Sep 10.
An accurate and sensitive analytical method has been developed for the quantification of genistein in dog plasma using high-performance liquid chromatography/tandem mass spectrometry. Genistein and diclofenac (internal standard) were extracted from the plasma sample using methyl tert-butyl ether and then separated on an Agilent Zorbax C18 column using a gradient mobile phase. The detector was a Q-trap mass spectrometer with an electrospray ionization interface operating in the multiple reaction monitoring mode. The assay was linear over the concentration range of 0.10-500 ng/mL with a lower limit of quantification of 0.10 ng/mL. The method was shown to be reproducible and reliable, with inter-day and intra-day accuracy and precision within ±15%. The method was successfully applied to a pharmacokinetic comparison of immediate and extended release tablets in beagle dogs after oral administration. Immediate release tablets showed rapid genistein absorption, with mean peak concentration of 726 ± 199 ng/mL reached at 0.2 ± 0.0 h. However, the absorption of genistein was considerably slower and more sustainable for extended release tablets. The relative bioavailability of the extended release tablet over the immediate release formulation was estimated to be 134 ± 47% based on the AUCInf values from non-compartmental analysis.
已开发出一种准确且灵敏的分析方法，用于使用高效液相色谱/串联质谱法定量犬血浆中的染料木黄酮。血浆样品中的染料木黄酮和双氯芬酸（内标）用甲基叔丁基醚萃取，然后在安捷伦Zorbax C18柱上使用梯度流动相进行分离。检测器为带有电喷雾电离接口的Q-阱质谱仪，以多反应监测模式运行。该测定法在0.10 - 500 ng/mL的浓度范围内呈线性，定量下限为0.10 ng/mL。该方法具有重现性和可靠性，日间和日内准确度及精密度在±15%以内。该方法成功应用于比格犬口服速释片和缓释片后的药代动力学比较。速释片显示染料木黄酮吸收迅速，在0.2 ± 0.0小时达到平均峰浓度726 ± 199 ng/mL。然而，缓释片对染料木黄酮的吸收明显较慢且更具持续性。基于非房室分析的AUCInf值，缓释片相对于速释制剂的相对生物利用度估计为134 ± 47%。
