GC-IMS Measurements of Synthetic and Human Urine for Quantitative VOC Analysis and Surrogate-Matrix Calibration

This dataset contains gas chromatography–ion mobility spectrometry (GC-IMS) measurements acquired from synthetic urine, pooled human urine, and individual urine samples. The dataset was generated in the context of research on quantitative volatile organic compound (VOC) analysis in urine using static headspace gas chromatography–ion mobility spectrometry (HS-GC-IMS), with a particular focus on surrogate-matrix calibration strategies for nonlinear detectors. Measurements were performed using a FlavourSpec GC-IMS instrument (G.A.S., Dortmund, Germany) equipped with a non-polar FS-SE-54-CB capillary column (30 m × 0.32 mm ID × 0.25 μm film thickness). The ion mobility spectrometer included a tritium ionization source and a 98 mm drift tube operating at an electric field of 500 V/cm. Nitrogen was used as both carrier and drift gas. Samples were analysed using static headspace injection. For each measurement, vials containing the sample matrix were incubated at 60 °C for 5 minutes, after which 300 μL of headspace were injected into the GC-IMS system using an automated sampler. Each GC-IMS acquisition produces a two-dimensional signal matrix representing ion intensity as a function of: chromatographic retention time ion mobility drift time Each measurement lasts 30 minutes of chromatographic acquisition time, followed by approximately 1.5 minutes of system cleaning and stabilization before the next run. During acquisition, IMS spectra are recorded at 30 ms intervals, and six scans are averaged per spectrum. As a result, each GC-IMS measurement contains approximately 4.5 million data points, providing high-resolution chromatographic and mobility information. The dataset contains multiple GC-IMS measurements corresponding to three matrices: synthetic urine, used as a surrogate calibration matrix pooled human urine, used as a reference matrix individual urine samples, used for quantitative evaluation Calibration experiments were performed over the concentration range 0–30 ppb for three volatile organic compounds: anisole 2-heptanone 2-pentanone Raw measurements are provided as instrument files in .mea format, generated by the FlavourSpec GC-IMS system. Each file contains the complete GC-IMS measurement including the ion current intensity matrix, acquisition parameters, and instrument metadata. To facilitate reproducible analysis, the dataset also includes: an annotation file linking each measurement to sample metadata (matrix type, acquisition time, batch, etc.) peak tables in CSV format derived from processed GC-IMS data for different sample categories Peak tables correspond to chromatographic-mobility peaks obtained after signal processing steps including denoising, alignment, peak detection, clustering, baseline correction, and peak integration using workflows implemented in the GC-IMS R package. The dataset is intended to support methodological research on: calibration strategies for nonlinear detectors matrix effects in headspace analysis GC-IMS signal processing workflows volatile metabolomics in urine quantitative VOC analysis in complex biological matrices The raw data provided here allow reconstruction and evaluation of GC-IMS processing pipelines and calibration workflows under controlled experimental conditions. To support transparency and reproducibility of the associated research, the dataset is made publicly available through this repository.