Kakkar T, Mayersohn M
Department of Pharmacy Practice and Science, and the Center for Toxicology, College of Pharmacy, University of Arizona, Tucson 85721, USA.
J Chromatogr B Biomed Sci Appl. 1998 Oct 23;718(1):69-75. doi: 10.1016/s0378-4347(98)00348-x.
A gas chromatographic-mass spectrometric (GC-MS) assay was developed for the quantitative analysis of methyl salicylate (MeS), ethyl salicylate (ES) and salicylic acid (SA) from biological fluids. The method was validated from 100-microl rat liver homogenate preparations (5 mg/ml protein) in 70 mM KH2PO4 (pH 7.4) buffer and from 100 microl rat plasma. The samples were extracted with chloroform, derivatized with BSTFA and quantitated by GC-MS in the SIM mode. The standard curves ranged from 31 ng/ml to 800 or 1250 ng/ml. Relative standard deviations and bias were less than 11% in plasma and homogenate for all compounds except SA which evidenced greater variability. The assay was used in preliminary experiments to characterize the pharmacokinetics of MeS in rats.
开发了一种气相色谱 - 质谱（GC-MS）分析法，用于定量分析生物流体中的水杨酸甲酯（MeS）、水杨酸乙酯（ES）和水杨酸（SA）。该方法在70 mM KH2PO4（pH 7.4）缓冲液中的100微升大鼠肝脏匀浆制剂（5 mg/ml蛋白质）以及100微升大鼠血浆中进行了验证。样品用氯仿萃取，用BSTFA衍生化，并通过GC-MS在选择离子监测（SIM）模式下进行定量。标准曲线范围为31 ng/ml至800或1250 ng/ml。除SA表现出较大变异性外，所有化合物在血浆和匀浆中的相对标准偏差和偏差均小于11%。该分析法用于初步实验以表征大鼠体内MeS的药代动力学。
