首页> 外文期刊>Therapeutic Drug Monitoring >Determination of buspirone and 1-(2-pyrimidinyl)-piperazine (1-PP) in human plasma by capillary gas chromatography.
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Determination of buspirone and 1-(2-pyrimidinyl)-piperazine (1-PP) in human plasma by capillary gas chromatography.

机译:毛细管气相色谱法测定人血浆中的丁螺环酮和1-(2-嘧啶基)-哌嗪(1-PP)。

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摘要

Two separate gas chromatographic methods for the determination of buspirone and its active metabolite, 1-(2-pyrimidinyl)-piperazine (1-PP) in human plasma are described. Both procedures involve solid-phase extraction (the packing material of the cartridges used was C8 for buspirone and a mixed-mode sorbent for 1-PP), injection of the sample into a gas chromatograph equipped with a fused-silica capillary column and a nitrogen-phosphorus detector, and analysis with temperature programming (from 220 degrees C to 285 degrees C for buspirone and from 138 degrees C to 285 degrees C for 1-PP). The coating material of the analytical column was 5% diphenyl dimethyl silicone for buspirone and 50% diphenyl dimethyl silicone for 1-PP. Zolpidem was used as an internal standard in the buspirone assay and 1-phenylpiperazine in the 1-PP assay. Recovery of buspirone and 1-PP averaged 98% and 89%, respectively, and the limit of quantification was 0.2 ng/mL for both compounds. The between-run coefficients of variation ranged from 3.2% to 9.4% and from 2.9% to 8.6% for samples spiked with three different concentrations of buspirone and 1-PP, respectively. The suitability of these assays for pharmacokinetic studies was shown by analyzing timed plasma samples from volunteers after ingestion of a single therapeutic dose of buspirone (10 mg).
机译:描述了测定人血浆中丁螺环酮及其活性代谢物1-(2-嘧啶基)-哌嗪(1-PP)的两种独立的气相色谱方法。两种方法都涉及固相萃取(丁螺环酮所用色谱柱的填充材料为C8,1-PP所用的色谱柱为混合模式吸附剂),将样品注入配有熔融石英毛细管柱和氮气的气相色谱仪中-磷检测器,并通过温度编程进行分析(丁螺环酮从220摄氏度到285摄氏度,1-PP从138摄氏度到285摄氏度)。分析柱的涂料是丁螺环酮的5%二苯基二甲基硅酮和1-PP的50%二苯基二甲基硅酮。唑吡坦在丁螺环酮测定中用作内标,在1-PP测定中用作1-苯基哌嗪。丁螺环酮和1-PP的回收率平均分别为98%和89%,两种化合物的定量限均为0.2 ng / mL。分别加有三种不同浓度的丁螺环酮和1-PP的样品的批间变异系数在3.2%至9.4%和2.9%至8.6%之间。摄入单一治疗剂量的丁螺环酮(10毫克)后,通过分析来自志愿者的定时血浆样品,证明了这些测定法对药代动力学研究的适用性。

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