An alternative derivatization method for the analysis of amino acids in cerebrospinal fluid by gas chromatography-mass spectrometry

作者：Nunes de Paiva Maria Jose; Menezes Helvecio Costa; Christo Paulo Pereira; Resende Rodrigo Ribeiro; Cardeal Zenilda de Lourdes^*

来源：Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2013, 931: 97-102.

DOI：10.1016/j.jchromb.2013.05.014

• L-Amino acids
• Microwave-assisted derivatization
• Gas chromatography
• Mass spectrometry

The determination of the concentrations of L-amino acids in cerebrospinal fluid (CSF) has been used to gain biochemical insight into central nervous system disorders. This paper describes a microwave-assisted derivatization (MAD) method using N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) as a derivatizing agent for determining the concentrations of L-amino acids in human CSF by gas chromatography with mass spectrometry (GC/MS). The experimental design used to optimize the conditions showed that the optimal derivatization time was 3 min with a microwave power of 210W. The method showed good performance for the validation parameters. The sensitivity was very good, with limits of detection (LODs) ranging from 0.01 mu mol L-1 to 4.24 mu mol L-1 and limits of quantification (LOQs) ranging from 0.02 to 7.07 mu mol L-1. The precision, measured using the relative standard deviation (RSD), ranged from 4.12 to 15.59% for intra-day analyses and from 6.36 to 18.71% for inter-day analyses. The coefficients of determination (R-2) were above 0.990 for all amino acids. The optimized and validated method was applied to the determination of amino acid concentrations in human CSF.

• 出版日期2013-7-15