Analysis of glutamine, glutamate, pyroglutamate, and GABA in cerebrospinal fluid using ion pairing HPLC with positive electrospray LC/MS/MS
Analysis of glutamine, glutamate, pyroglutamate, and GABA in cerebrospinal fluid using ion pairing HPLC with positive electrospray LC/MS/MS
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DOI：
10.1016/j.jneumeth.2008.02.019
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发表时间：
2008-06-30
影响因子：
3
通讯作者：
Ackermann, Bradley L.
中科院分区：
文献类型：
--
作者：
Eckstein, James A.;Ammerman, Gina M.;Ackermann, Bradley L.
提出了一种简单、灵敏的脑脊液 (CSF) 中谷氨酰胺、谷氨酸、焦谷氨酸和 γ-氨基丁酸 (GABA) 的分离和定量方法。该方法利用与七氟丁酸 (HFBA) 的离子对实现 HPLC 分离，并通过正 ESI LC/MS/MS 进行检测。该方法不需要提取或衍生化，对每种分析物使用重标记内标，并可在 5 分钟运行时间内实现快速通量。该方法的开发特别注意防止已知分析物在某些条件下发生的转化。所有分析物的定量下限为 7.8 ng/ml，并且为所有分析物定义了日内和日间准确度 (%RE) 和精密度 (%R.S.D.)。该方法被开发为一种灵敏、选择性和稳健的方法，用于研究兴奋性和抑制性神经递质（谷氨酸和 GABA）作为药物开发中的生物标志物。 (c) 2008 Elsevier B.V. 保留所有权利。
A simple and sensitive method for the separation and quantitation of glutamine, glutamate, pyroglutamate, and gamma-aminobutyric acid (GABA) in cerebrospinal fluid (CSF) is presented. The method utilizes ion pairing with heptafluorobutyric acid (HFBA) to achieve HPLC separation with detection by positive ESI LC/MS/MS. The method does not require extraction or derivatization, utilizes a heavy labeled internal standard for each analyte, and allows for rapid throughput with a 5 min run time. The method was developed with particular attention taken to prevent conversion between analytes known to occur under certain conditions. The lower limit of quantitation is 7.8 ng/ml for all analytes, and the intro-day and inter-day accuracy (%RE) and precision (%R.S.D.) are defined for all analytes. The method was developed as a sensitive, selective, and robust method to investigate the excitatory and inhibitory neurotransmitters (glutamate and GABA) as biomarkers in drug development. (c) 2008 Elsevier B.V. All rights reserved.