Journal
EUROPEAN JOURNAL OF CANCER
Volume 50, Issue 11, Pages 1993-2002Publisher
ELSEVIER SCI LTD
DOI: 10.1016/j.ejca.2014.04.011
Keywords
Urine; Volatile metabolomic profile; Renal cell carcinoma; Central composite design; Headspace solid-phase microextraction; Gas chromatography-ion trap/mass spectrometry
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Funding
- European Union (FEDER funds through COMPETE)
- National Funds (FCT, Fundacao para a Ciencia e Tecnologia) [Pest-C/EQB/LA0006/2013]
- FCT [SFRH/BD/80518/2011]
- Fundação para a Ciência e a Tecnologia [SFRH/BD/80518/2011] Funding Source: FCT
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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/poly-dimethylsiloxane (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 degrees 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. (C) 2014 Elsevier Ltd. All rights reserved.
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