Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008, Salamanca, Spain.
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008, Salamanca, Spain.
Talanta. 2020 Feb 1;208:120381. doi: 10.1016/j.talanta.2019.120381. Epub 2019 Sep 20.
Amino acids have been of great interest in clinical studies since variation in their concentration may provide information about different disorders. For the first time, a non-separative method based on single quadrupole mass spectrometry (qMS) for the simultaneous semiquantitative determination of sixteen amino acids in saliva samples has been developed. The method includes derivatisation of amino acids with ethyl chloroformate-pyridine-ethanol to obtain volatile products, liquid-liquid extraction (LLE) and further analysis using a programmed temperature vaporizer (PTV) coupled to qMS. This method could be applied to the analysis of a great number of saliva samples, limiting the use of separative methods only when abnormal concentrations of amino acids were found, reducing analysis time and cost. The results obtained in the determination of amino acids using the non-separative method were compared to those obtained when a separative method based on gas chromatography (GC) was used, providing values of average relative predictive error (E %) ranging between 2 and 48%. Repeatability and reproducibility were tested, obtaining relative standard deviation (RSD) values equal to or lower than 11% and 16%, respectively. Detection limits were in the range of 0.076-8.747 mg L for the non-separative method.
自氨基酸浓度的变化可能提供有关不同疾病的信息以来,它们一直是临床研究中的热点。本文首次建立了一种基于单四极杆质谱(qMS)的非分离方法,用于同时半定量测定唾液样本中的十六种氨基酸。该方法包括用氯甲酸乙酯-吡啶-乙醇衍生氨基酸以获得挥发性产物,液液萃取(LLE),然后使用程序升温汽化器(PTV)与 qMS 进一步分析。该方法可应用于大量唾液样本的分析,仅在发现氨基酸浓度异常时才使用分离方法,从而减少分析时间和成本。使用非分离方法测定氨基酸的结果与使用基于气相色谱(GC)的分离方法的结果进行了比较,平均相对预测误差(E%)值在 2%至 48%之间。对重复性和再现性进行了测试,得到的相对标准偏差(RSD)值分别等于或低于 11%和 16%。非分离方法的检测限范围为 0.076-8.747 mg/L。