High performance liquid chromatographic determination of mazindol in human plasma.

High performance liquid chromatographic determination of mazindol in human plasma.
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高效液相色谱法测定人血浆中马吲哚的含量。

DOI:
10.1039/b106008m
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发表时间:
2001
期刊:
The Analyst
影响因子:
--
通讯作者:
K. Nakashima
K. Nakashima
中科院分区:
--
文献类型:
--
作者:
A. Kaddoumi;M. Mori;K. Nanashima;M. Kono;K. Nakashima

文献摘要

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建立了简便高效的紫外检测液相色谱法测定人血浆中马辛吲哚[5-(对氯苯基)-2,5-二氢- 3h -咪唑[2,1- A]异吲哚-5-醇]及其主要代谢物2-(2-氨基乙基)-3-(对氯苯基)-3-羟基邻苯二胺(Met)的含量。用乙酸乙酯从血浆样品中提取分析物,在C18柱上以乙腈-0.067 mol dm(-3)磷酸盐缓冲液(pH 3.5) (24 + 76 v/v)为流动相分离。在220 nm处监测洗脱液。经过完整的验证和稳定性研究,该方法被证明是敏感和精确的。mazindol和Met的检出限分别为0.07和0.08 ng ml(-1)。两种化合物的准确度和回收率分别为94 ~ 102%和91 ~ 102%。两种化合物的分析精密度分别小于7.6%和9.2%。考察了不同贮藏条件下(室温、4℃、冻融循环)的稳定性。在室温和4℃下的血浆样品中,Mazindol是不稳定的。本方法应用于用Mazindol治疗肥胖症患者血浆中Mazindol和Met的测定。
A simple and convenient high performance liquid chromatographic method with UV detection is described for the determination of mazindol [5-(p-chlorophenyl)-2,5-dihydro-3H-imidazo[2,1-a]isoindol-5-ol] and its major metabolite, 2-(2-aminoethyl)-3-(p-chlorophenyl)-3-hydroxyphthalimidine (Met), in human plasma. The analytes were extracted with ethyl acetate from plasma samples and separated on a C18 column using acetonitrile-0.067 mol dm(-3) phosphate buffer (pH 3.5) (24 + 76 v/v) as a mobile phase. The eluates were monitored at 220 nm. Following complete validation and stability studies, the proposed method proved to be sensitive and precise. The limits of detection were 0.07 and 0.08 ng ml(-1) of plasma for mazindol and Met, respectively. The accuracy and recovery were in the ranges 94-102% and 91-102%, respectively, for both compounds. The intra- and inter-assay precisions were less than 7.6 and 9.2%, respectively, for both compounds. The stability of mazindol under different storage conditions, i.e., at room temperature (rt) and 4 degrees C and with freeze-thaw cycles, was also examined. Mazindol was unstable in plasma samples left at rt and 4 degrees C. The method was applied to the determination of mazindol and Met in the plasma of a patient treated for obesity with mazindol.