Analysis of volatile human urinary metabolome by solid-phase microextraction in combination with gas chromatography-mass spectrometry for biomarker discovery: application in a pilot study to discriminate patients with renal cell carcinoma

Márcia Monteiro*, Márcia Carvalho, Rui Henrique, Carmen Jerónimo, Nathalie Moreira, Maria de Lourdes Bastos, Paula Guedes de Pinho

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

57 Citations (Scopus)

Abstract

A new and simple analytical approach consisting of headspace-solid phase microextraction (HS-SPME) sampling coupled with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed to study the volatile human urinary metabolome. A central composite design (CCD) was used in the optimisation of extraction conditions. Fibre selection and evaluation of pH influence were performed using an univariate mode and the influence of other parameters, such as the time and temperature of extraction, time of incubation and salt addition, that affect the efficiency of the SPME sampling, was carried out using a CCD. With a sample volume of 2 mL, the optimal conditions in terms of total response values and reproducibility were achieved by performing analyses with a divinylbenzene/polydimethylsiloxane (DVB/PDMS) fibre, in an acidic pH (pH 2) with the addition of 0.59 g of NaCl, allowing the sample to equilibrate for 9 min and extracting at 68 °C for 24 min. The applicability of the optimised method was then tested in a pilot non-target analysis of urine samples obtained from patients with renal cell carcinoma (RCC) and healthy individuals. Chemometric unsupervised analyses performed on the volatile pattern acquired for these samples clearly showed the potential of volatile urinary metabolome to discriminate between RCC and control patients.
Original languageEnglish
Pages (from-to)1993-2002
Number of pages10
JournalEuropean Journal of Cancer
Volume50
Issue number11
DOIs
Publication statusPublished - Jul 2014

Keywords

  • Central composite design
  • Gas chromatography-ion trap/mass spectrometry
  • Headspace solid-phase microextraction
  • Renal cell carcinoma
  • Urine
  • Volatile metabolomic profile

Fingerprint

Dive into the research topics of 'Analysis of volatile human urinary metabolome by solid-phase microextraction in combination with gas chromatography-mass spectrometry for biomarker discovery: application in a pilot study to discriminate patients with renal cell carcinoma'. Together they form a unique fingerprint.

Cite this