Development of an arrow solid-phase microextraction GC-MS/MS method for the determination of 69 odorants in water

A quantitative method for determining 69 odorants in water was developed using arrow-type headspace solid-phase microextraction (SPME) coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Key extraction parameters, including extraction and desorption temperatures and times, NaCl addition, fiber type, and rotation speed, were systematically optimized. Under the optimized conditions, target compounds were efficiently enriched, separated on a polar chromatographic column, detected in selected reaction monitoring (SRM) mode, and quantified using external calibration. The method demonstrated high sensitivity, with limits of detection (LODs) ranging from 0.015 to 75 ng/L, and 55 compounds exhibiting LODs below 10 ng/L. All analytes showed excellent linearity (R² > 0.995) within their respective ranges. Precision was satisfactory, with relative standard deviations (RSDs) between 1.10 % and 17.85 %, including 59 compounds with RSDs <10 %. Average recoveries at three spiking levels ranged from 80 % to 120 %. This automated and environmentally friendly method offers high sensitivity and accuracy, meeting the analytical requirements for complex odorants in water.