Validated analytical method to determine new salivary lipid peroxidation compounds as potential neurodegenerative biomarkers

J Pharm Biomed Anal. 2019 Feb 5:164:742-749. doi: 10.1016/j.jpba.2018.11.043. Epub 2018 Nov 19.

Abstract

Lipid peroxidation is closely related to neurodegenerative diseases since brain shows high lipid composition and oxygen consumption. The determination of lipid peroxidation compounds in non-invasive biological samples would help to monitor the patients' oxidative stress status. A new analytical method based on ultrasound-assisted liquid-liquid semi-microextraction (UA-LLsME) followed by Ultra Performance Liquid Chromatography coupled to tandem Mass Spectrometry was developed to determine 18 lipid peroxidation biomarkers in saliva samples. The variables affecting the UA-LLsME efficiency were systematically studied. Under the optimum conditions, the methodology was validated and showed high-throughput, high sensitivity (limits of detection 0.02-2 nmol L-1), and satisfactory precision (coefficients of variation 2-11% (intra-day) and 5-12% (inter-day)). The reliability of the described method was assessed analysing spiked saliva samples, and the recoveries were between 80% and 120% for most of the analytes. Then, the method suitability was demonstrated by analysing saliva samples (n = 30) from elderly people with neurodegenerative diseases. To conclude, the new developed analytical method is a useful tool to determine salivary lipid peroxidation compounds as potential biomarkers in further clinical studies in which oxidative stress plays an important role.

Keywords: Isoprostanes; Lipid peroxidation; Liquid-liquid microextraction; Mass spectrometry; saliva.

Publication types

  • Validation Study

MeSH terms

  • Aged
  • Biomarkers / analysis
  • Chromatography, High Pressure Liquid / instrumentation
  • Chromatography, High Pressure Liquid / methods
  • Female
  • Humans
  • Limit of Detection
  • Lipid Peroxidation*
  • Lipids / analysis*
  • Liquid Phase Microextraction / instrumentation
  • Liquid Phase Microextraction / methods*
  • Male
  • Middle Aged
  • Neurodegenerative Diseases / diagnosis*
  • Neurodegenerative Diseases / metabolism
  • Oxidative Stress
  • Reproducibility of Results
  • Saliva / chemistry*
  • Tandem Mass Spectrometry / instrumentation
  • Tandem Mass Spectrometry / methods
  • Ultrasonic Waves

Substances

  • Biomarkers
  • Lipids