Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products

An efficient sample preparation method using gas-diffusion microextraction (GDME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) is proposed for the first time to determine fragrance allergens in both aqueous and alcohol-based cosmetic products. The most significant GD...

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Main Authors: Ana Castiñeira-Landeira, Angel Gomez-Feas, Antonia M. Carro, Thierry Dagnac, Paulo J. Almeida, Maria Llompart
Format: Article
Language:English
Published: Elsevier 2025-05-01
Series:Advances in Sample Preparation
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Online Access:http://www.sciencedirect.com/science/article/pii/S2772582025000403
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author Ana Castiñeira-Landeira
Angel Gomez-Feas
Antonia M. Carro
Thierry Dagnac
Paulo J. Almeida
Maria Llompart
author_facet Ana Castiñeira-Landeira
Angel Gomez-Feas
Antonia M. Carro
Thierry Dagnac
Paulo J. Almeida
Maria Llompart
author_sort Ana Castiñeira-Landeira
collection DOAJ
description An efficient sample preparation method using gas-diffusion microextraction (GDME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) is proposed for the first time to determine fragrance allergens in both aqueous and alcohol-based cosmetic products. The most significant GDME parameters were optimized, starting with extraction temperature as a preliminary experiment. Subsequently, an experimental design was performed to evaluate the influence of six parameters: acceptor solution volume, acetonitrile percentage in the acceptor solution, sample dilution, salting-out effect, extraction time, and sample volume. Under the optimized conditions, the method was validated in terms of linearity, precision, trueness, obtaining a good performance. The validated methodology was applied to twelve real cosmetic samples, demonstrating the widespread occurrence of these allergens in cosmetics. Notably, lilial, a compound prohibited by Regulation EC No 1223/2009, was detected in one cosmetic product (460 μg mL-1); and the concentrations of some of the target fragrance allergens in some samples reach values above 1000 μg mL-1. This methodology represents a sustainable and practical approach, supported by AGREEPrep and BAGI metrics, respectively.
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spelling doaj-art-22b59e6f75a8436c9fab0388f4f92ccf2025-08-20T01:51:53ZengElsevierAdvances in Sample Preparation2772-58202025-05-011410018710.1016/j.sampre.2025.100187Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic productsAna Castiñeira-Landeira0Angel Gomez-Feas1Antonia M. Carro2Thierry Dagnac3Paulo J. Almeida4Maria Llompart5CRETUS, Department of Analytical Chemistry, Nutrition and Food Science, Universidade de Santiago de Compostela E-15782 Santiago de Compostela, SpainCRETUS, Department of Analytical Chemistry, Nutrition and Food Science, Universidade de Santiago de Compostela E-15782 Santiago de Compostela, SpainIMATUS, IDIS, Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, Universidade de Santiago de Compostela E-15782 Santiago de Compostela, SpainAgronomic and Agricultural Research Centre (AGACAL-CIAM), Unit of Organic Contaminants, P.O. Box 10 E-15080 A Coruña, SpainREQUIMTE/LAQV – Departamento de Química e Bioquímica, Faculdade de Ciências da Universidade do Porto, 4169-007, Porto, PortugalCRETUS, Department of Analytical Chemistry, Nutrition and Food Science, Universidade de Santiago de Compostela E-15782 Santiago de Compostela, Spain; Corresponding author.An efficient sample preparation method using gas-diffusion microextraction (GDME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) is proposed for the first time to determine fragrance allergens in both aqueous and alcohol-based cosmetic products. The most significant GDME parameters were optimized, starting with extraction temperature as a preliminary experiment. Subsequently, an experimental design was performed to evaluate the influence of six parameters: acceptor solution volume, acetonitrile percentage in the acceptor solution, sample dilution, salting-out effect, extraction time, and sample volume. Under the optimized conditions, the method was validated in terms of linearity, precision, trueness, obtaining a good performance. The validated methodology was applied to twelve real cosmetic samples, demonstrating the widespread occurrence of these allergens in cosmetics. Notably, lilial, a compound prohibited by Regulation EC No 1223/2009, was detected in one cosmetic product (460 μg mL-1); and the concentrations of some of the target fragrance allergens in some samples reach values above 1000 μg mL-1. This methodology represents a sustainable and practical approach, supported by AGREEPrep and BAGI metrics, respectively.http://www.sciencedirect.com/science/article/pii/S2772582025000403GDMEGC–MS/MSFragrance allergensCosmetic productsSample preparationAnalytical metrics
spellingShingle Ana Castiñeira-Landeira
Angel Gomez-Feas
Antonia M. Carro
Thierry Dagnac
Paulo J. Almeida
Maria Llompart
Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
Advances in Sample Preparation
GDME
GC–MS/MS
Fragrance allergens
Cosmetic products
Sample preparation
Analytical metrics
title Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
title_full Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
title_fullStr Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
title_full_unstemmed Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
title_short Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
title_sort novel gas diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products
topic GDME
GC–MS/MS
Fragrance allergens
Cosmetic products
Sample preparation
Analytical metrics
url http://www.sciencedirect.com/science/article/pii/S2772582025000403
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