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Here, we present a quantitative method for H 2 detection by gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) using a single quadrupole instrument. Additionally, the developed method was applied to the detection of H 2 in human blood by GC-SIM-MS analysis using the existing 22 Ne in air as an internal standard (IS). H 2 was analyzed by GC-SIM-MS using a single quadrupole instrument with double TC-Molsieve 5A capillary columns for the separation of permanent gases. The detections of H 2 (analyte) and 22 Ne (IS) were performed at m/z 2 and 22, respectively, by GC-SIM-MS. The analyte and IS were separated using He as the carrier gas. The ratio of the peak area of H 2 to 22 Ne was employed to obtain a calibration curve for H 2 determination in the gas phase. The proposed GC-SIM-MS method exhibited high sensitivity in terms of the limits of detection (LOD) (1.7 ppm) and quantitation (LOQ) (5.8 ppm) for H 2 analysis. The developed quantitative assay of H 2 in the headspace of blood samples achieved high repeatability with a relative standard deviation (RSD) of 1.4 - 4.7%. We successfully detected and quantified H 2 in the headspaces of vacuum blood-collection tubes containing whole blood from 11 deceased individuals with several causes of death by employing the developed GC-SIM-MS method. The quantitative value of H 2 ranged from 5 to 905 ppm. The proposed GC-SIM-MS method was applicable to the quantitative assay of H 2 in biological samples without tedious pretreatment requirements.

Quantitative Determination of H2 in Human Blood by 22Ne-aided Gas Chromatography-Mass Spectrometry Using a Single Quadrupole Instrument