Journal Highlight: Determination of cyclic volatile methylsiloxanes in personal care products by gas chromatography

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  • Published: Dec 11, 2017
  • Author: separationsNOW
  • Channels: Gas Chromatography
thumbnail image: Journal Highlight: Determination of cyclic volatile methylsiloxanes in personal care products by gas chromatography

A simple GC-FID method has been developed to enable accurate measurement of low levels of octamethylcyclotetrasiloxane (D4) and decamethylcyclotetrasiloxane (D5) in personal care products.

Determination of cyclic volatile methylsiloxanes in personal care products by gas chromatography

International Journal of Cosmetic Science, 2017, 39, 580-588
H. M. Brothers Jr, T. Boehmer, R. A. Campbell, S. Dorn, J. J. Kerbleski, S. Lewis, C. Mund, D. Pero, K. Saito, M. Wieser W. Zoller

Abstract: A simple analytical method has been developed to enable accurate measurement of octamethylcyclotetrasiloxane (D4) and decamethylcyclotetrasiloxane (D5) down to the circa 0.1 weight per cent level in personal care products. Although gas chromatography methods are reported in the literature for quantitation of D4 and D5 in several matrices including PCPs, the potential for generation of false positives due to contamination, co-elution and in situ generation of cyclic volatile methylsiloxanes (cVMS) is always present and needs to be controlled. This report demonstrates the applicability of using a combination of emulsion break, liquid–liquid extraction and silylation sample preparation followed by GC-FID analysis as a suitable means of analysing PCPs for specific cVMS. The reliability and limitations of such methodology were demonstrated through several round-robin studies conducted in the laboratories of a consortium of silicone manufacturers. In addition, this report presents examples of false positives encountered during development of the method and presents a comparative analysis between this method and a published QuEChERS sample preparation procedure to illustrate the potential for generation of false positives when an inappropriate approach is applied to determination of cVMS in personal care products. This report demonstrates that an approach to determine cVMS levels in personal care products is to perform an emulsion break on the sample, isolate the non-polar phase from the emulsion break and treat with a silylation reagent to abate potential in situ formation of cyclics during the course of GC-FID analysis. Round-robin studies conducted in laboratories representing multiple siloxane manufacturers demonstrated the reliability of the GC-FID method when measuring cVMS in PCPs down to circa 0.1%.

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