Development, validation, and assessment of a reliable and white method for the analysis of water-based perfumes by pipette-tip micro-solid-phase extraction combined with dual detection gas chromatography

The analysis of possible allergens, impurities, and contaminants in perfumes and the determination of their volatile fingerprints are of high importance in determining their quality. At the same time, the analysis of perfumes with a significant water content can require complex procedures or large amounts of material. These new products are becoming increasingly popular as they reduce skin dryness and irritation, but they require the addition of additives to improve the solubility of all fragrance components. Direct injection into gas chromatography can lead to interferences and requires more frequent maintenance of the chromatographic system, while traditional extraction methods need several steps, a large volume of sample and material, and the use of toxic solvents. In this study, pipette-tip micro-solid-phase extraction (PT-µSPE) was used and optimized as an innovative, simple, sustainable, and time-saving approach. It requires only 10 mg Celite and 10 mg sample while elution is carried out with 100 mg heptane/ethyl acetate (70/30, p/p). The extraction is coupled with GC analysis with simultaneous FID and MS detection (GC-MS/FID), which is used for qualitative, semi-quantitative, and quantitative purposes. The performance of the PT-µSPE method was validated and successfully applied to commercial samples. In addition, the performance of the developed method and of the reference approaches was evaluated, focusing mainly on the overall impact of analysis in accordance with the principles of White Analytical Chemistry. The results show that the PT-µSPE method is more balanced than the conventional methods in terms of analytical performance, greenness, and practical efficiency, making it a valuable alternative for routine use in the fragrance industry.