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首页> 外文期刊>Analytica chimica acta >Development of C60-based labeling reagents for the determination of low-molecular-weight compounds by matrix assisted laser desorption ionization mass spectrometry (II): Determination of thiols in human serum
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Development of C60-based labeling reagents for the determination of low-molecular-weight compounds by matrix assisted laser desorption ionization mass spectrometry (II): Determination of thiols in human serum

机译：基于C60的标记试剂通过基质辅助激光解吸电离质谱法测定低分子量化合物的标记试剂：人血清中硫醇的测定

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摘要

Perturbation of thiol homeostasis in biological fluids are thought to be associated with several diseases, and reliable analytical methods for the determination of low molecular weight (LMW) thiols in human plasma or serum are thus required. In this study, a matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) method is described for high throughput determination of four LMW thiols (glutathione, cysteine, homocysteine and cysteinylglycine) in human serum. It is based on the use of a bromoacetyl functionalized C60 (Br-C60) as a derivatization reagent to label thiols. The Br-C60 labeling can add an 832-Da tag to thiols, which moves thiol signals to high mass region and effectively avoids the signal interference generated by the traditional MALDI matrix below 800 Da. The labeling can be completed within 5 min under microwave-assisted condition. Thereby, the Br-C60 labeling based MALDI-TOF MS analytical method can achieve high throughput analysis of LMW thiols in serum. Good linearities of the method for the thiols in human serum were obtained in the range of 0.5-500.0 mu M with correlation coefficient (R) greater than 0.9960. The limit of detection is in the range of 0.07-0.18 mu M for the investigated thiols in human serum with relative standard deviations of lower than 13.5% and recoveries ranging from 81.9 to 117.1%. Using the method, four thiols in microliter serum samples of breast cancer (BC) patients were determined. The result showed that the contents of the four thiols in BC serum samples significantly changed compared to the healthy control (HC). (C) 2020 Elsevier B.V. All rights reserved.
机译：认为，生物液中硫醇稳态的扰动被认为是与几种疾病相关的，因此需要用于测定人血浆或血清中的低分子量（LMW）硫醇的可靠分析方法。在该研究中，用于在人血清中的四种LMW硫醇（谷胱甘肽，半胱氨酸，半胱氨酸和半胱氨酸）的高通量测定，描述了基质辅助激光解吸/电离飞行时间质谱（MALDI-TOF MS）方法。它基于使用溴代乙酰官能化C60（BR-C60）作为标记硫醇的衍生化试剂。 BR-C60标记可以向硫醇添加832-DA标签，其将硫醇信号移动到高质量区域，并有效地避免了由传统的MALDI矩阵产生的信号干扰在800da以下。标记可以在微波辅助条件下在5分钟内完成。由此，基于BR-C60标记的MALDI-TOF MS分析方法可以在血清中实现LMW硫醇的高通量分析。人血清中硫醇方法的良好线性在0.5-500.0μm的范围内，相关系数（r）大于0.9960。对于人血清中的研究硫醇的检测限为0.07-0.18μm，具有低于13.5％的相对标准偏差，回收率为81.9至117.1％。使用该方法，确定了乳腺癌（BC）患者的微升血清样品中的四个硫醇。结果表明，与健康对照（HC）相比，BC血清样品中的四个硫醇的含量显着变化。 （c）2020 Elsevier B.V.保留所有权利。

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