Routine quantification of 54 allergens in fragrances using comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry with dual parallel secondary columns. Part I: Method development

The forthcoming extension of the regulated fragrance allergen number is raising a challenge: the previously developed quantification methods need to be drastically improved in terms of rapidity, without altering their reliability. This work describes a procedure based on comprehensive bidimensional gas chromatography, hyphenated with a low‐cost quadrupole mass spectrometer (GCxGC‐QMS). The second chromatographic dimension was operated in a dual configuration, consisting of two parallel secondary columns, one being connected to the QMS, the other to a flame ionization detector (FID). This not only allowed optimization of the chromatographic gas flows when compared to the usual single second dimension, but it also enabled the use of the FID signal to extend the quantification range from 2 to 10,000 mg/kg. The QMS was used at a low level (2‐100 mg/kg), where coelutions are frequent, and the FID was used for the most abundant analytes (100‐10,000 mg/kg) with a low risk of significant interferences. To assess the identity and purity of the analyte peak at low level, we propose a strategy and summarize it in a decisional tree. To our knowledge, this represents the first fully developed quantification method based on a GCx2GC‐QMS/FID system. In contrast to other methods, it enables the quantification of a wide variety of analytes in fragrances in a single run, without requiring a series of sample dilutions to match the calibration range.