Quantifying exhaled acetone and isoprene through solid phase microextraction and gas chromatography-mass spectrometry

• Published in: Analytica chimica acta Vol. 1301; p. 342468
• Main Authors: Schulz, Eray, Woollam, Mark, Vashistha, Sneha, Agarwal, Mangilal
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01.05.2024
• Subjects: Exhaled breath; Gas chromatography; Mass spectrometry; Quantification; Solid phase microextraction; Volatile organic compound; Solid phase microextraction; Gas chromatography; Volatile organic compound; Quantification; Mass spectrometry; Exhaled breath
• ISSN: 0003-2670; 1873-4324; 1873-4324
• DOI: 10.1016/j.aca.2024.342468

Acetone, isoprene, and other volatile organic compounds (VOCs) in exhaled breath have been shown to be biomarkers for many medical conditions. Researchers use different techniques for VOC detection, including solid phase microextraction (SPME), to preconcentrate volatile analytes prior to instrumental analysis by gas chromatography-mass spectrometry (GC-MS). These techniques include a previously developed method to detect VOCs in breath directly using SPME, but it is uncommon for studies to quantify exhaled volatiles because it can be time consuming due to the need of many external/internal standards, and there is no standardized or widely accepted method. The objective of this study was to develop an accessible method to quantify acetone and isoprene in breath by SPME GC-MS. A system was developed to mimic human exhalation and expose VOCs to a SPME fiber in the gas phase at known concentrations. VOCs were bubbled/diluted with dry air at a fixed flow rate, duration, and volume that was comparable to a previously developed breath sampling method. Identification of acetone and isoprene through GC-MS was verified using standards and observing overlaps in chromatographic retention/mass spectral fragmentation. Calibration curves were developed for these two analytes, which showed a high degree of linear correlation. Acetone and isoprene displayed limits of detection/quantification equal to 12 ppb/37 ppb and 73 ppb/222 ppb respectively. Quantification results in healthy breath samples (n = 15) showed acetone concentrations spanned between 71 ppb and 294 ppb, and isoprene varied between 170 ppb and 990 ppb. Both concentration ranges for acetone and isoprene in this study overlap with those reported in existing literature. Results indicate the development of a system to quantify acetone and isoprene in breath that can be adapted to diverse sampling methods and instrumental analyses beyond SPME GC-MS. [Display omitted] •There are no standardized or widely available methods for exhaled VOC quantification.•A system was developed for quantifying exhaled VOCs by SPME GC-MS.•Calibration curves generated to quantify isoprene/acetone in human subjects.•The method is easily adaptable to other sampling techniques.•Strides made toward analytical validation and quantification.