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采用柱前衍生化高效液相色谱法和荧光检测法测定人血浆中的白消安。

Determination of busulfan in human plasma using high-performance liquid chromatography with pre-column derivatization and fluorescence detection.

作者信息

Peris J E, Latorre J A, Castel V, Verdeguer A, Esteve S, Torres-Molina F

机构信息

Departamento de Farmacia y Tecnología Farmacéutica, Facultad de Farmacia, Universidad de Valencia, Spain.

出版信息

J Chromatogr B Biomed Sci Appl. 1999 Jun 25;730(1):33-40. doi: 10.1016/s0378-4347(99)00214-5.

DOI:10.1016/s0378-4347(99)00214-5
PMID:10437669
Abstract

A rapid, sensitive and reproducible high-performance liquid chromatographic assay for busulfan in human plasma was developed. After extraction of plasma samples with acetonitrile and methylene chloride, busulfan and the internal standard [1,5-bis(methanesulfonyloxy)pentane] were derivatized with 8-mercaptoquinoline to yield fluorescent compounds which were detected with a fluorescence detector equipped with filters of 360 nm (excitation) and 425 nm (emission). Calibration graphs showed a linear correlation (r>0.9990) over the concentration range of 20-2000 ng/ml. The recovery of busulfan from plasma standards was 70+/-5%. The detection and quantification limits for busulfan in plasma samples were established at 9 ng/ml and 20 ng/ml, respectively. The intra- and inter-assay variations were lower than 8% and 10%, respectively. The applicability of the method was verified by analyzing the plasma concentrations of busulfan in a patient to whom it was administered orally on two different days.

摘要

建立了一种快速、灵敏且可重复的人血浆中白消安的高效液相色谱测定法。用乙腈和二氯甲烷萃取血浆样品后,白消安和内标物[1,5-双(甲磺酰氧基)戊烷]用8-巯基喹啉衍生化,生成荧光化合物,用配备360nm(激发)和425nm(发射)滤光片的荧光检测器进行检测。校准曲线在20-2000ng/ml的浓度范围内呈线性相关(r>0.9990)。血浆标准品中白消安的回收率为70±5%。血浆样品中白消安的检测限和定量限分别确定为9ng/ml和20ng/ml。批内和批间变异分别低于8%和10%。通过分析在两天不同时间口服白消安的患者的血浆浓度,验证了该方法的适用性。

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