A sensitive gas chromatography-mass spectrometry (GC–MS) method has been developed and validated for the detection and quantification of 1,8-Cineol in tissue samples of nasal polyps from CRSwNP patients.
The analytes were chromatographically separated on a fused silica column with 95% dimethyl and 5% diphenyl polysiloxane (Rtx-5 Amine; 30 m, 0,25 mm ID, 0,25 µm film-thickness; Restek Corporation, Bellefonte, PA, USA) using a 6890N with MSD 5973 Network gas chromatography mass spectrometry system (Agilent Technologies Inc., Santa Clara, CA, USA). The temperature program used for chromatographic separation is described in Table 1. Helium (5.0, Messer GmbH, Bad Soden am Taunus, Germany) at a constant flow of 1.5 mL/min was used as a carrier gas. Electron ionization (EI) at 70 eV was used at a source temperature of 230 °C. Mass spectrometric determination was performed in selective ion monitoring (SIM) mode, analyzing the masses m/z 154 (used for quantification) and m/z 108 as a qualifier for 1,8-Cineol. Quantifier and qualifier mass transitions for 1,4-Cineol were m/z 111 and m/z 154, respectively. MS quadrupole temperature was 150 °C. A solvent delay of 4 min was used with following acquisition for 10 min.

Temperature program of the gas chromatograph.

Ramp noRate [°C/min]End temperature [°C]Time [min]
Start0502
1201300
2302500
Post-run02902
MassHunter GC/MS Acquisition (B.07.06.2704, Agilent Technologies. Inc. Santa Clara, CA, USA) and MassHunter Workstation Quantitative Analysis (B.09.00) were employed for data acquisition and evaluation.
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