Improving the Speed and Quantitative Performance for the Analysis of Allergenic and Carcinogenic Dyes in Industrial, Cosmetics, Personal Care and Consumer Products

Importance of the Topic

Dyes are extensively incorporated into industrial, cosmetic, personal care, and consumer products to enhance appearance and marketability. Certain disperse, acid, direct, and basic dyes exhibit allergenic or carcinogenic properties, prompting regulatory restrictions and risk assessments. Rapid, sensitive, and selective analytical methods are critical for ensuring compliance with restricted substances lists and safeguarding public health and the environment.

Objectives and Study Overview

This study presents a streamlined approach for the simultaneous identification and quantification of 24 allergenic and carcinogenic dyes in textiles and consumer goods. The primary goals are to increase sample throughput, improve sensitivity and selectivity, reduce solvent consumption, and demonstrate method robustness compared to conventional HPLC or TLC protocols.

Methodology and Instrumentation

Textile samples (0.5 g) were extracted with methanol in an ultrasonic bath and diluted prior to analysis. Chromatographic separation was performed on an ACQUITY UPLC BEH C18 column (2.1×50 mm, 1.7 µm) at 30 °C using a 7 min gradient from 10 % to 95 % acetonitrile in water (both containing 5 mmol/L ammonium acetate) at 0.6 mL/min. Detection employed a Xevo TQD tandem quadrupole mass spectrometer in fast polarity-switching MRM mode, with optimized cone voltages and collision energies for each dye.

Used Instrumentation

• Waters ACQUITY UPLC H-Class System
• Waters Xevo TQD tandem quadrupole MS
• MassLynx and TargetLynx software
• ACQUITY UPLC BEH C18 column (2.1×50 mm, 1.7 µm)

Main Results and Discussion

Transitioning from HPLC (17 min run) to UPLC (7 min run) reduced analysis time by over 60% and solvent use by 86%. The fast cycle and polarity switching of the Xevo TQD resolved narrow UPLC peaks with increased signal-to-noise ratios. Calibration curves (0.01–1.5 µg/mL) exhibited excellent linearity across compounds. Spiked textile recoveries at 30 and 75 µg/g ranged from 91% to 110% with RSDs below 5%.

Benefits and Practical Applications

• Over fivefold increase in sample throughput compared to HPLC
• Significant solvent savings and lower running costs
• Enhanced sensitivity and selectivity for allergenic and carcinogenic dyes
• Single-injection analysis of positive and negative ions
• Robust quantification suitable for regulatory compliance and quality control in textiles and consumer products

Future Trends and Opportunities

Emerging directions include integration of high-resolution MS for structural confirmation, further miniaturization of chromatography, automation of sample preparation, expansion of target lists to novel synthetic dyes, and adoption of green solvent systems to reduce environmental impact.

Conclusion

The combined ACQUITY UPLC H-Class and Xevo TQD solution delivers a fast, reliable, and cost-effective platform for the quantitative analysis of allergenic and carcinogenic dyes. Method migration tools and optimized MRM conditions ensure seamless transition from legacy HPLC methods while meeting stringent regulatory requirements.

References

1. BS EN 71-9:2005+A1:2007 Safety of toys—Organic chemical compounds. European Committee for Standardization.
2. Sustainable Textile Production (STeP). OEKO-TEX Association; accessed October 2015.
3. Commission Decision 2009/567/EC establishing ecological criteria for the EU Ecolabel for textile products. Official Journal L197, 2009.
4. Regulation (EC) No 1223/2009 on cosmetic products. Official Journal L342, 2009.
5. DIN 54231:2005 Textiles—Detection of dispersed dyestuffs. German Institute for Standardization.
6. Lord GA, Gordon DB, Tetler LW, Carr CM. Electrochromatography–electrospray mass spectrometry of textile dyes. J Chromatogr A. 1995;700:27–33.
7. Qiang M, Hua B, Qing Z, Wei M, et al. Determination of carcinogenic and allergenic dyestuffs in toys by LC–UV/VIS and tandem MS. Chromatographia. 2010;72:85–93.
8. Morgan S, Vann B, Baguley B, Stefan A. Advances in discrimination of dyed textile fibers using capillary electrophoresis/MS. Proc. FBI Trace Evidence Symposium. 2007.
9. Ràfols C, Barceló D. Determination of mono- and disulphonated azo dyes by LC–APCI-MS. J Chromatogr A. 1997;777:177–192.
10. Holčapek M, Jandera P, Příkryl J. Analysis of sulphonated dyes by ESI-MS. Dyes Pigments. 1999;43:127–137.
11. Socher G, Nussbaum R, Rissler K, Lankmayr E. Analysis of sulfonated compounds by ion-exchange HPLC-MS. J Chromatogr A. 2001;912:53–60.
12. Waters reversed-phase column selectivity chart. Waters Corporation; accessed 2012.
13. Craven K. HPLC to UPLC Method Migration Using Acrylate Analysis as a Model. Waters Application Note 720004105en. 2011.