DETERMINATION OF CHLORPHENIRAMINE IN HUMAN BLOOD SERUM

氯苯那敏的检测方法 正在开发血清以支持将要进行的临床研究 在Paul Turkeltaub医学博士的指导下，免疫生物化学实验室， DAPP，CBER。一个已经过评估和部分验证的程序， 包括萃取、浓缩和气相色谱法。 扑尔敏是通过选择性离子监测质谱检测 特征碎片离子的m/e值为203 提取效率和 注射体积通过加入四氘代 扑尔敏和监测类似的D4碎片离子在m/e 207. 开发一种替代方法， 扑尔敏的对映体成分，正在进行中。 使用气相色谱法尚未获得对映体拆分 手性柱 基于α-糖蛋白的HPLC色谱柱， β-环糊精固定相提供了对映体拆分， 但是还没有实现在ppb水平上检测扑尔敏 通过UV吸光度。 尚未评价其他HPLC检测方法， 提供必要的灵敏度。 一个前专栏的工作正在进行中 涉及与氯甲酸苄酯反应的手性衍生化方法 HPLC和荧光检测可提供必要的灵敏度 用于检测血清平衡水平的扑尔敏， 允许对映体物种形成。

The determination of chlorpheniramine at low part per billion levels in blood serum is being developed to support a clinical study to be conducted under the direction of Paul Turkeltaub, M.D., Lab of Immunobiochemistry, DAPP, CBER. One procedure, that has been evaluated and partially validated, involves extraction, concentration and gas chromatography. Chlorpheniramine is detected by selective ion monitoring mass spectrometry of a characteristic fragment ion at m/e 203. Extraction efficiency and injection volume are normalized by addition of tetradeuterated chlorpheniramine and monitoring of the analogous D4 fragment ion at m/e 207. Development of an alternate method, that would permit the resolution of chlorpheniramine into its enantiometic components, is in progress. Enantiomeric resolution has not been obtained using gas chromatographic chiral columns. HPLC columns based on alpha-glycoprotein and beta-cyclodextrin stationary phases have provided enantiomeric resolution, but detection of chlorpheniramine at ppb levels has not been accomplished by UV absorbance. Other HPLC detection methods have not been evaluated as providing necessary sensitivity. Work is in progress on a pre-column derivatization method involving reaction with benzylchloroformate, chiral HPLC and fluorescence detection that may provide the necessary sensitivity for detection of chlorpheniramine at serum equilibrium levels while allowing enantiomeric speciation.