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Headspace Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry for the Determination of Volatile Organic Compounds in Urine

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Abstract

Determination of volatile organic compounds (VOCs), the metabolites produced in human body, contributes to better understanding of the mechanisms responsible for the progression of diseases and facilitates monitoring of the responses to treatment. Urine samples are a rich source of VOCs and they constitute a non-invasive tool for diagnosis of various metabolic and pathological states. The aim of this study was to optimize the headspace solid-phase microextraction coupled with gas chromatography−mass spectrometry (HS-SPME−GC/MS) method for analysis of urine samples on the example of urine collected from children with celiac disease. Pooled urine samples from three children with celiac disease were used to select the optimal fibers, time and temperature of extraction, salt dose, and pH to achieve the highest SPME efficiency. Analysis performed with the use of divinylbenzene/carboxen/polydimethylsiloxane fiber in acidic pH with the addition of 1.5 g of sodium chloride supported the extraction of the highest number of VOCs with the largest total peak area. The extraction conducted at 60°C for 45 min led to an optimal improvement in efficiency with a reduced number of siloxane derivatives, indicative of degradation of septa, fiber, and/or GC column stationary phase. The optimized HS-SPME−GC/MS method can be successfully applied to the determination of VOCs in urine samples.

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Funding

The research was supported by statutory funds of the Department of Chemistry and Biodynamics of Food in the Institute of Animal Reproduction and Food Research PAS and by the National Science Centre, Poland (project no. 2016/21/N/NZ9/01510).

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Authors and Affiliations

  1. Department of Chemistry and Biodynamics of Food, Institute of Animal Reproduction and Food Research of Polish Academy of Sciences, 10-747, Olsztyn, Poland

    Natalia Drabińska, Małgorzata Starowicz & Urszula Krupa-Kozak

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  1. Natalia Drabińska
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  2. Małgorzata Starowicz
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  3. Urszula Krupa-Kozak
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Correspondence to Małgorzata Starowicz.

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Natalia Drabińska, Starowicz, M. & Krupa-Kozak, U. Headspace Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry for the Determination of Volatile Organic Compounds in Urine. J Anal Chem 75, 792–801 (2020). https://doi.org/10.1134/S1061934820060088

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  • DOI: https://doi.org/10.1134/S1061934820060088

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