采用毛细管气相色谱-质谱联用技术同时定量测定人血浆和尿液中丁螺环酮及1-(2-嘧啶基)哌嗪的含量。

Simultaneous quantitation of buspirone and 1-(2-pyrimidinyl)piperazine in human plasma and urine by capillary gas chromatography-mass spectrometry.

作者信息

Sciacca M A, Duncan G F, Shea J P, Faulkner H C, Farmen R H, Pittman K A

机构信息

Department of Metabolism and Pharmackinetics, Bristol-Myers Company, Syracuse, NY 13221.

出版信息

J Chromatogr. 1988 Jul 15;428(2):265-74. doi: 10.1016/s0378-4347(00)83917-1.

DOI:10.1016/s0378-4347(00)83917-1

PMID:3215930

Abstract

Buspirone and a buspirone metabolite, 1-(2-pyrimidinyl)piperazine (1-PP), are extracted from matrix using C18 extraction columns. The metabolite and its internal standard (d4-1-PP) are derivatized with pentafluorobenzoyl chloride to the corresponding amides. The 1-PP derivatives, buspirone and the buspirone internal standard (5-fluorobuspirone) are co-chromatographed. Chromatography and detection are performed using capillary gas chromatography with a fused-silica column and selected-ion monitoring-mass spectrometry. Linear range of the standard curves in plasma is 0.1-14 ng/ml for buspirone and 0.2-25 ng/ml for 1-PP with lower limits of quantitation of 0.1 and 0.2 ng/ml, respectively. In urine the linear range of the standard curves is 0.2-14 ng/ml for buspirone and 8-500 ng/ml for 1-PP with lower limits of quantitation of 0.2 and 8.0 ng/ml, respectively. Intra-assay accuracies were within 14% for buspirone and 1-PP in plasma and urine. Intra-assay precision was within 12% for both compounds in both matrices.

摘要

丁螺环酮及其代谢物1-(2-嘧啶基)哌嗪(1-PP)采用C18萃取柱从基质中萃取。代谢物及其内标(d4-1-PP)用五氟苯甲酰氯衍生为相应的酰胺。1-PP衍生物、丁螺环酮和丁螺环酮内标(5-氟丁螺环酮)进行共色谱分析。使用带有熔融石英柱的毛细管气相色谱和选择离子监测质谱进行色谱分析和检测。血浆中丁螺环酮标准曲线的线性范围为0.1-14 ng/ml，1-PP为0.2-25 ng/ml，定量下限分别为0.1和0.2 ng/ml。在尿液中，丁螺环酮标准曲线的线性范围为0.2-14 ng/ml，1-PP为8-500 ng/ml，定量下限分别为0.2和8.0 ng/ml。丁螺环酮和1-PP在血浆和尿液中的批内准确度在14%以内。两种化合物在两种基质中的批内精密度均在12%以内。