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Determination of plasma ziprasidone using liquid chromatography with fluorescence detection

机译:液相色谱-荧光检测法测定血浆齐拉西酮

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A liquid chromatographic procedure was developed for the determination of a new antipsychotic agent ziprasidone in plasma using fluorescence detection. A one-step liquid–liquid extraction from 1 ml of alkalinized plasma containing an internal standard α-ergocryptine using methyl-t-butyl ether afforded a greater than 84% recovery of ziprasidone. Chromatography was performed using a reversed-phase trimethylsilyl bonded silica column with a mobile phase of 72:28 phosphate buffer:acetonitrile at a flow rate of 1.5 ml/min. Detection of the eluted peaks was observed using excitation and emission wavelengths of 320 and 410 nm, respectively. Chromatographic run time did not exceed 14 min with no interference from endogenous material. The calibration curve was linear over the concentration range of 0.5 to 200 ng/ml and the inter- and intra-assay imprecision (CV) was less than 10%. The lower limit of quantitation was assessed at 0.5 ng/ml. Specificity of the method is demonstrated by the lack of interference from a large number of commonly used drugs and their metabolites in clinical use. The utility of the method is exemplified with the presentation of clinical data from patients receiving ziprasidone.
机译:开发了一种液相色谱程序,用于使用荧光检测法测定血浆中的新型抗精神病药齐拉西酮。使用甲基叔丁基醚从1毫升含内标α-麦角隐碱的碱化血浆中进行一步法液-液萃取,可获得高于41%的齐拉西酮回收率。使用反相三甲基甲硅烷基键合硅胶色谱柱,流动相为72:28磷酸盐缓冲液:乙腈,以1.5 ml / min的流速进行色谱分离。分别使用320和410 nm的激发和发射波长观察到洗脱峰的检测。色谱运行时间不超过14分钟,且不受内源物质的干扰。校准曲线在0.5至200 ng / ml的浓度范围内是线性的,批间和批内不准确性(CV)小于10%。定量下限为0.5 ng / ml。该方法的特异性通过在临床使用中不受大量常用药物及其代谢产物的干扰来证明。该方法的效用以接受齐拉西酮的患者的临床数据呈现为例。

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