Four-stage (low-)flow modulation comprehensive gas chromatography-quadrupole mass spectrometry for the determination of recently-highlighted cosmetic allergens

Abstract

The present research is based on the development and use of a flow-modulation (FM) comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GC×GC-qMS) method for the determination of recently-highlighted (by the Scientific Committee on Consumer Safety) fragrance allergens (54) in cosmetics. FM GC×GC-qMS conditions were finely tuned to generate flow conditions (≈7 mL min(-1)) compatible with the qMS system used. Six-point calibration curves, over the range 1, 5, 10, 20, 50, 100 mg L(-1), were constructed for the 54 target allergens, with satisfactory linearity observed in all cases. Absolute quantification was performed by using extracted ions; target analyte identification was performed through measurement of ion ratios (qualifier/quantifier), full-scan MS database matching and the use of linear retention indices. Additional analytical figures of merit subjected to measurement were intra-day repeatability, accuracy at the 25 and 5 mg L(-1) levels, and limits of detection and quantification. The number of data points per peak, along with mass spectral skewing, was also subjected to evaluation. Finally, the FM GC×GC-qMS method was used not only for the quantification of target allergens in five commercial perfumes, but also for general qualitative profiling.

Keywords: Comprehensive two-dimensional gas chromatography; Flow modulation; Fragrance allergens; Perfumes; Quadrupole mass spectrometry.