ANALYTICAL METHOD FOR QUANTITATION OF BREFELDIN A IN MOUSE PLASMA

开发了一种专门的、灵敏的分析方法 小鼠血浆中灯盏花素A(89671)的定量测定。 该方法采用毛细管气-液色谱， 电子俘获探测。发现了商业上可用的1-二十烷醇 作为一个合适的内标。药物和内标分别为 用乙醚从50pl血浆中提取，用 蒸发和用全氟酰化试剂处理的残留物 产生捕获电子的衍生品。导数的等分 然后将混合物引入熔融二氧化硅毛细管柱， 墙面涂有交联型甲基硅胶。从中国排出的污水 用~(63)Ni电子捕获监测的气相色谱柱 探测器。通过绘制峰面积比，绘制标准曲线 以灯盏花素A为内标，对照灯盏花素A。 集中精神。用最小二乘法确定了最佳拟合直线 用倒数峰面积加权因子进行平方回归 平方计算斜率、y截距和相关系数。 未知样品中的Brefeldin A浓度使用 回归分析结果。该物质的浓度范围 本检测方法从0.1微克/毫升延伸到2.2微克/毫升，并且 在该范围内，其精密度和准确度为10%或更高。较低的 定量限为0.1微克/毫升，而最低限量为 检出量约为0.025微克/毫升。当今的毛细管气 层析分析法适合于初步研究。 灯盏花素A在小鼠体内的药代动力学。

A specific, sensitive analytical method was developed for the quantitative determination of brefeldin A (NSC 89671) in mouse plasma. The assay utilizes capillary gas-liquid chromatography with electron-capture detection. Commercially available 1-eicosanol was found to be a suitable internal standard. The drug and internal standard were extracted from 50 pl of plasma with diethyl ether, the solvent removed by evaporation and the residue treated with a perfluoroacylating reagent to yield the electron-capturing derivatives. Aliquots of the derivative mixtures were then introduced onto a fused silica capillary column, which is wall-coated with cross-linked methyl silicone gum. The effluent from the gas chromatographic column as monitored using a 63Ni electron capture detector. Standard curves were prepared by plotting peak area ratios of brefeldin A to the internal standard against the brefeldin A concentration. The best fit straight line was determined by least squares regression using a weighting factor of reciprocal peak area squared to calculate the slope, y-intercept and correlation coefficient. Brefeldin A concentrations in unknown samples were calculated using the results of the regression analysis. The concentration range of the present assay extends from 0.1 micrograms/ML to 2.2 micrograms/ML, and its precision and accuracy over that range are 10% or better. The lower limit of quantitation is 0.1 micrograms/mL, while the lower limit of detection is about 0.025 micrograms/mL. The present capillary gas chromatographic assay is appropriate for the preliminary investigation of brefeldin A pharmacokinetics in mice.