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采用简单的 GC-MS 方法,直接在血斑上衍生化,测定干血斑中的γ-羟基丁酸。

Determination of gamma-hydroxybutyric acid in dried blood spots using a simple GC-MS method with direct "on spot" derivatization.

机构信息

Laboratory of Toxicology, Faculty of Pharmaceutical Sciences, Ghent University, Harelbekestraat 72, 9000 Ghent, Belgium.

出版信息

Anal Bioanal Chem. 2010 Nov;398(5):2173-82. doi: 10.1007/s00216-010-4183-9. Epub 2010 Sep 12.

Abstract

The objective of this study was the development of an accurate and sensitive method for the determination of gamma-hydroxybutyric acid (GHB) in dried whole blood samples using a GC-MS method. The complete procedure was optimized, with special attention on the sample pretreatment, and validated. Therefore, dried blood spots of only 50 μl were prepared and, after the addition of internal standard GHB-d6, directly derivatized using 100 μl of a freshly prepared mixture of trifluoroacetic acid anhydride and heptafluorobutanol (2:1). The derivatized extract was injected into a gas chromatograph coupled to a mass spectrometer (GC-MS), operating in the electron impact mode, with a total run time of 12.3 min. Method validation included the evaluation of linearity, precision, accuracy, sensitivity, selectivity, and stability. A weighting factor of 1/x(2) was chosen and acceptable intra-batch precision, inter-batch precision, and accuracy were seen. The linear calibration curve ranged from 2 to 100 μg/ml, with a limit of detection of 1 μg/ml. Our procedure, utilizing the novel approach of direct "on spot" derivatization followed by analysis with GC-MS, proved to be reliable, fast, and applicable in routine toxicology.

摘要

本研究的目的是开发一种准确、灵敏的 GC-MS 法测定全血干血斑中 γ-羟基丁酸(GHB)的方法。对整个过程进行了优化,特别注意样品预处理,并进行了验证。因此,仅制备了 50μl 的干血斑,然后加入内标 GHB-d6,直接用 100μl 新鲜制备的三氟乙酸酐和七氟丁醇(2:1)混合物衍生化。衍生化提取物注入配有质量光谱仪(GC-MS)的气相色谱仪中,以电子冲击模式运行,总运行时间为 12.3 分钟。方法验证包括线性、精密度、准确度、灵敏度、选择性和稳定性的评价。选择了权重因子 1/x(2),并观察到可接受的批内精密度、批间精密度和准确度。线性校准曲线范围为 2 至 100μg/ml,检测限为 1μg/ml。我们的方法采用直接“点上”衍生化,然后用 GC-MS 进行分析的新方法,证明是可靠、快速且适用于常规毒物学分析的。

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