Rapid Screening of Skin Lightening Products for the Corticosteroid Clobetasol Propionate Using Direct Analysis in Real Time (DART) with Mass Detection

Importance of the Topic

Unauthorized inclusion of corticosteroids such as clobetasol propionate in skin lightening cosmetics poses significant health risks due to long term adverse effects including skin atrophy and systemic conditions. Rapid screening methods are essential to protect consumers and enforce regulatory standards.

Objectives and Study Overview

This study aimed to develop a fast and reliable technique for detecting clobetasol propionate in cosmetic products. By leveraging direct analysis in real time coupled with mass detection, the goal was to eliminate extensive sample preparation and chromatography while achieving qualitative confirmation of active pharmaceutical ingredients and common additives.

Methodology and Instrumentation

Ambient desorption ionization was performed using a DART source in negative mode with a helium gas stream heated to 350 C and an ACQUITY QDa mass detector. Sampling was conducted on QuickStrip cards at 1 mm/s. Data acquisition and control were managed with MassLynx and the DART interface software.

• DART source (IonSense) with heated helium at 350 C
• ACQUITY QDa mass detector in negative ion mode
• MassLynx MS and DART interface software
• QuickStrip cards for direct sample introduction

Main Results and Discussion

Clobetasol propionate was detected as an [M-H]- ion at m/z 465 with a characteristic chlorine isotope pattern in both cream (0.05% w/w declared) and gel samples. Arbutin ([M-H]- at m/z 271) and parabens such as methyl, ethyl, propyl, and butyl parabens (m/z 151, 165, 179, 193) were also identified. Spectral subtraction facilitated clear differentiation between solvent standards and real samples, confirming the presence of undeclared corticosteroids and labeled ingredients.

Benefits and Practical Applications

This approach offers rapid qualitative screening without solvent extraction or chromatographic separation, reducing analysis time and resource requirements. It is suitable for routine quality control, regulatory surveillance, and preliminary investigation of cosmetic products for banned or undeclared active ingredients.

Future Trends and Opportunities

Further refinement could include quantitative methods using LC-MS for positive samples, expansion to other prohibited actives, and development of portable ambient MS systems for on-site inspections. Integration with advanced data processing and machine learning may enhance detection sensitivity and throughput.

Conclusion

DART-MS using an ACQUITY QDa detector provides an efficient and reliable screening tool for detecting clobetasol propionate and other additives in cosmetic products. This method supports rapid decision making in regulatory and quality control settings and complements more detailed confirmatory analyses.

References

1. Desmedt B Courselle P De Beer JO Rogiers V Deconinck E De Paepe K Illegal cosmetics on the EU market a threat for human health Arch Toxicol 88 1765–1766 2014
2. Desmedt B Van Hoeck E Rogiers V Courselle P De Beer JO De Paepe K Deconinck E Characterisation of suspected illegal skin whitening cosmetics J Pharm Biomed Anal 90 85–91 2014
3. Desmedt B Courselle P De Beer JO Rogiers V Grosber M Deconinck E De Paepe K Overview of skin whitening agents with insight into the illegal cosmetic market JEADV 30 943–950 2016
4. Fiori J Andrisane V LC-MS method for simultaneous determination of glucocorticoids in pharmaceutical formulations and counterfeit cosmetics J Pharm Biomed Anal 91 185–192 2014
5. Sik Nam Y Kwon KI Lee KB Monitoring of clobetasol propionate and betamethasone dipropionate as undeclared steroids in cosmetic products Forensic Sci Intl 210 144–148 2011
6. EU Regulation 1223/2009 2009
7. FDA Hydroquinone Studies Under The National Toxicology Program NTP 2016
8. Cody R Laramee J Durst H Versatile new ion source for analysis of materials in open air under ambient conditions Anal Chem 77 2297–2302 2005
9. Van Berkel GJ Pasilis SP Ovchinnikova O Established and emerging atmospheric pressure surface sampling techniques J Mass Spec 43 1163–1180 2008
10. Wells JM Roth MJ Keil AD Grossenbacher JW Justes DR Patterson GE Barket DJ Implementation of DART and DESI on a fieldable MS JASMS 19 1419–1424 2008
11. Haunschmidt M Buchberger W Klampfl CK Hertsens R Identification and semiquantitation of parabens and UV filters by DART MS Anal Methods 3 99–104 2011
12. Ma Q Bai H Li W Wang C Li X Cooks GR Direct identification of prohibited substances in cosmetics and foodstuffs using ambient ionization Anal Chim Acta 912 65–73 2016
13. Cabaleiro N de la Calle I Bendicho C Lavilla I Sample preparation for determination of parabens in cosmetics Trends Anal Chem 57 34–46 2014
14. Twohig M Cooper J Stumpf C Identification of skin lightening agents using ACQUITY Arc with PDA mass detection Waters Application Note 2016