顶空固相微萃取结合气相色谱/正离子化学电离质谱法测定血浆和尿液中的γ-羟基丁酸

Determination of gamma-hydroxybutyric acid (GHB) in plasma and urine by headspace solid-phase microextraction and gas chromatography/positive ion chemical ionization mass spectrometry.

作者信息

Frison G, Tedeschi L, Maietti S, Ferrara S D

机构信息

Forensic Toxicology and Antidoping, University Hospital of Padova, Via Falloppio 50, I-35121 Padova, Italy.

出版信息

Rapid Commun Mass Spectrom. 2000;14(24):2401-7. doi: 10.1002/1097-0231(20001230)14:24<2401::AID-RCM179>3.0.CO;2-I.

DOI:10.1002/1097-0231(20001230)14:24<2401::AID-RCM179>3.0.CO;2-I

PMID:11114057

Abstract

A new method for the qualitative and quantitative analysis of gamma-hydroxybutyric acid (GHB) in plasma and urine samples is described. It involves the conversion of GHB to gamma-butyrolactone (GBL), its subsequent headspace solid-phase microextraction (SPME), and detection by gas chromatography/positive ion chemical ionization mass spectrometry (GC/PICI-MS), using D(6)-GBL as internal standard. The assay is linear over a plasma GHB range of 1-100 microg/mL (n = 5, r = 0.999) and a urine GHB range of 5-150 microg/mL (n = 5, r = 0. 998). Relative intra- and inter-assay standard deviations, determined for plasma and urine samples at 5 and 50 microg/mL, are all below 5%. The method is simple, specific and reasonably fast. It may be applied for clinical and forensic toxicology as well as for purposes of therapeutic drug monitoring.

摘要

本文描述了一种用于血浆和尿液样本中γ-羟基丁酸（GHB）定性和定量分析的新方法。该方法包括将GHB转化为γ-丁内酯（GBL），随后进行顶空固相微萃取（SPME），并以D(6)-GBL作为内标，通过气相色谱/正离子化学电离质谱（GC/PICI-MS）进行检测。该测定法在血浆GHB浓度范围为1-100μg/mL（n = 5，r = 0.999）和尿液GHB浓度范围为5-150μg/mL（n = 5，r = 0.998）内呈线性。在5μg/mL和50μg/mL浓度下对血浆和尿液样本测定的相对批内和批间标准差均低于5%。该方法简单、特异且速度适中。可应用于临床和法医毒理学以及治疗药物监测。