气相色谱-质谱联用法定量分析血浆中羟基脲的三甲基硅烷基衍生物

Quantitative analysis of trimethylsilyl derivative of hydroxyurea in plasma by gas chromatography-mass spectrometry.

作者信息

James Hutchinson, Nahavandi Masoud, Wyche Melville Q, Taylor Robert E

机构信息

Department of Pharmacology, College of Medicine, Howard University, 520 W Street N.W., Washington, DC 20059, USA.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Feb 2;831(1-2):42-7. doi: 10.1016/j.jchromb.2005.11.033. Epub 2005 Dec 27.

DOI:10.1016/j.jchromb.2005.11.033

PMID:16378766

Abstract

Hydroxyurea is an antitumor drug widely used in the treatment of sickle cell disease. The drug has been analyzed in biological fluids by a number of high-performance liquid chromatography (HPLC) methods. This paper describes a fast and highly reliable capillary gas chromatography-mass spectrometry (GC-MS) procedure that was developed for the detection and quantitation of hydroxyurea in plasma. The compound and its labeled internal standard were liquid extracted from plasma and derivatized with BSTFA before analysis. The detection limit of the assay was 0.078 microg/ml and the limit of quantitation was 0.313 microg/ml with linearity up to 500 microg/ml. Intra-day variation, as coefficient of variation (C.V., %) over the selected concentration range, was 0.3-8.7% and inter-day variation was 0.4-9.6%.

摘要

羟基脲是一种广泛用于治疗镰状细胞病的抗肿瘤药物。已有多种高效液相色谱（HPLC）方法用于分析生物流体中的该药物。本文描述了一种快速且高度可靠的毛细管气相色谱-质谱（GC-MS）方法，该方法用于检测和定量血浆中的羟基脲。在分析前，该化合物及其标记的内标从血浆中进行液液萃取并用BSTFA衍生化。该测定法的检测限为0.078微克/毫升，定量限为0.313微克/毫升，线性范围高达500微克/毫升。在所选择的浓度范围内，日内变异以变异系数（C.V.，%）计为0.3 - 8.7%，日间变异为0.4 - 9.6%。