Metabolic profiling of aromatic compounds in cerebrospinal fluid of neurosurgical patients using microextraction by packed sorbent and liquid-liquid extraction with gas chromatography-mass spectrometry analysis

Biomed Chromatogr. 2021 Feb;35(2):e4969. doi: 10.1002/bmc.4969. Epub 2020 Sep 9.

Abstract

A new approach to the quantitative analysis of aromatic metabolites in cerebrospinal fluid samples of neurosurgical patients based on microextraction by packed sorbent coupled with derivatization and GC-MS was developed. Analytical characteristics such as recoveries (40-90%), limit of detection (0.1-0.3 μm) and limit of quantitation (0.4-0.7 μm) values, accuracy (<±20%), precision (<20%) and linear correlations (R2 ≥ 0.99) over a 0.4-10 μm range of concentrations demonstrated that microextraction by packed sorbent provides results for the quantitative analysis of target compounds comparable with those for liquid-liquid extraction. Similar results were achieved using 40 μl of sample for microextraction by packed sorbent instead of 200 μl for liquid-liquid extraction. Benzoic, 3-phenylpropionic, 3-phenyllactic, 4-hydroxybenzoic, 2-(4-hydroxyphenyl)acetic, homovanillic and 3-(4-hydroxyphenyl)lactic acids were found in cerebrospinal fluid samples (n = 138) of neurosurgical patients in lower concentrations than in serum samples (n = 110) of critically ill patients. Analysis of the cerebrospinal fluid and serum samples taken at the same time from neurosurgical patients (n = 5) revealed similar results for patients without infection and multidirectional results for patients with central nervous system infection. Our preliminary results demonstrate the necessity of further evaluating the aromatic compound profile in cerebrospinal fluid for its subsequent verification for potential diagnostic markers.

Keywords: aromatic metabolites; cerebrospinal fluid; gas chromatography-mass spectrometry; liquid-liquid extraction; microextraction by packed sorbent; neurosurgical patients.

MeSH terms

  • Adult
  • Carboxylic Acids / cerebrospinal fluid*
  • Carboxylic Acids / chemistry
  • Carboxylic Acids / isolation & purification
  • Carboxylic Acids / metabolism*
  • Female
  • Gas Chromatography-Mass Spectrometry / methods*
  • Humans
  • Limit of Detection
  • Linear Models
  • Liquid-Liquid Extraction / methods*
  • Male
  • Middle Aged
  • Reproducibility of Results

Substances

  • Carboxylic Acids