一种快速有效的 GC-MS/MS 方法，用于同时定量检测血清肌醇和 D-chiro 肌醇异构体。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A Pub Date : 2024-08-08 DOI:10.1016/j.chroma.2024.465246

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引用次数: 0

摘要

背景：肌醇（MI）和D-肌醇（DCI）是肌醇的两种重要异构体，在葡萄糖和类固醇代谢中都至关重要。MI、DCI或MI/DCI比值的缺失与多种病理过程密切相关，而MI和DCI在人体标本中缺乏实际测量：方法：为了同时定量检测血清样本中的 MI 和 DCI，建立了气相色谱串联质谱（GC-MS/MS）方法。优化了离子源、衍生剂用量和反应时间等工艺流程。结果：该方法灵敏度高（LOD ≤ 30 ng/mL of MI, ≤ 3 ng/mL of DCI），重现性好（重复分析时 RSD < 6 %）。MI 和 DCI 的定量测定在 0.500-10.00 和 0.005-0.500 μg/mL 的测量范围内线性良好（R2 > 0.999）。MI和DCI的回收率分别为97.11-99.35%和107.82-113.09%。该方法成功应用于114份临床样本。在当前条件下，血清样本中未观察到明显的基质效应。

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A rapid and validated GC-MS/MS method for simultaneous quantification of serum Myo- and D-chiro-inositol isomers

Background

Myo-inositol (MI) and D-chiro-inositol (DCI) are two paramount isomers of inositol, both vital in glucose and steroid metabolism. Deficits in MI, DCI or MI/DCI ratio are expressly concerned with several pathological process, whereas MI and DCI lack practical measurement for human specimen.

Methods

To quantify MI and DCI in serum samples simultaneously, a gas chromatography tandem mass spectrometry (GC-MS/MS) method was established. The process flow was optimized in ion source, derivative agent volume and reaction time. The performance characteristics were verified by commercial standards and clinical serums.

Results

This method was confirmed to be sensitive (LOD ≤ 30 ng/mL of MI, ≤3 ng/mL of DCI) and reproducible (RSD < 6 % for repeated analyses). Quantitative determinations performed good linearity within the measurement range of 0.500–10.00 and 0.005–0.500 μg/mL for MI and DCI respectively (R² > 0.999). The recoveries of MI and DCI were 97.11–99.35 % and 107.82–113.09 %, respectively. This method was successfully applied to 114 clinical specimens. No significant matrix effect was observed in serum samples under current conditions.

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来源期刊

Journal of Chromatography A 化学-分析化学

CiteScore

7.90

自引率

14.60%

发文量

742

审稿时长

45 days

期刊介绍： The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.