Development of a screening and confirmatory method for the analysis of polar endogenous compounds in saliva based on a liquid chromatographic-tandem mass spectrometric system
Development of a screening and confirmatory method for the analysis of polar endogenous compounds in saliva based on a liquid chromatographic-tandem mass spectrometric system
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DOI：
10.1016/j.chroma.2019.01.001
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发表时间：
2019-04-12
影响因子：
4.1
通讯作者：
Luis Perez-Pavon, Jose
中科院分区：
文献类型：
--
作者：
Teresa Fernandez-del-Campo-Garcia, Maria;Maria Casas-Ferreira, Ana;Luis Perez-Pavon, Jose
本文提出了一种高通量的方法，用于唾液中极性化合物的灵敏筛选和确证分析，该方法基于与三重四极杆质谱仪耦合的液相色谱系统的两步法。在这两个步骤中都使用了反相色谱柱，流动相组成的变化允许使用相同的仪器配置进行筛选和确证分析。建议的策略已被测试用于测定唾液样本中的多种极性内源性化合物(肌酸、多胺和氨基酸)。对整个过程的验证表明，两个步骤中所有化合物的结果都是一致的。对两种方法的重复性和重复性进行了评估，重复性情况下的重复性值低于8%，重复性情况下的重复性值小于17%。肌氨酸和赖氨酸的仪器检出限分别在1.22×10~(-3)~46.1×10~(-3)mg/L之间，以表观回收率为指标评价方法的准确度，结果在80~127%之间。对基质效应进行了评价，发现样品的基质对分析结果有影响。因此，采用一点标准加入法进行定量。将优化的两步法应用于表面健康的志愿者的唾液样本。总体而言，这两个步骤都获得了令人满意的结果，证明了该方法在此类基质中极性内源化合物的定量分析中的适用性。(C)2019爱思唯尔B.V.保留所有权利。
In this paper, a high-throughput approach is proposed for the sensitive screening and the confirmatory analysis of polar compounds in saliva using a two-step approach based on a liquid chromatographic system coupled to a triple quadrupole mass spectrometer. A reversed-phase chromatographic column was used in both steps and changes in the composition of the mobile phase allowed the screening and the confirmatory analyses to be performed with the same instrumental configuration. The proposed strategy has been tested for the determination of a multiclass group of polar endogenous compounds (creatinine, polyamines and amino acids) in saliva samples. The validation of the entire procedure showed consistent results for all the compounds in both steps. Repeatability and reproducibility were evaluated for both procedures, with values below 8% in the case of repeatability and 17% in the case of reproducibility. The instrumental limits of detection were found to be between 1.22 x 10(-3) and 46.1 x 10(-3) mg/L for creatinine and lysine, respectively, and accuracy of the method was evaluated in terms of apparent recoveries and values were found to be between 80 and 127%. Matrix effects were evaluated and it was found that the analytical outcome was influenced by the matrix of the sample. Thus, a one-point standard addition method was used for quantification. The optimized two-step procedure was applied to saliva samples from apparent healthy volunteers. Overall, satisfactory results were obtained in both steps, demonstrating its applicability for quantitative analysis of polar endogenous compounds in this kind of matrices. (C) 2019 Elsevier B.V. All rights reserved.