Quantitative determination of octadecenedioic acid in human skin and transdermal perfusates by gas chromatography-mass spectrometry.

Abstract

A gas chromatographic (GC) method with mass spectrometric (MS) detection is developed and validated for the accurate and precise determination of octadecenedioic acid (C18:1 DIOIC) in human skin samples and transdermal perfusates. C18:1 DIOIC is extracted using methanol. The saturated analogue 1,18-octadecanedioic acid (C18:0 DIOIC) is added as internal standard. Prior to analysis, both compounds are converted to their trimethylsilylated derivatives using N,O-bis(trimethylsilyl)trifluoroacetamide with 15% trimethylchlorosilane. Quantitation is performed in selected ion monitoring mode with a limit of quantitation of 250 ng/mL. Linearity with a correlation coefficient of 0.998 is obtained over a concentration range of 250-2000 ng/mL. Values for within-day accuracy range from 94.5% to 102.4%, and from 97.5% to 105.8% for between-day accuracy. Within- and between-day precision values are better than 5% and 7%, respectively. The recovery values from the various matrices vary from 92.6% to 104.0%. The GC-MS method is employed for the determination of C18:1 DIOIC after application of an emulsion containing the active ingredient onto human skin in vitro. The results demonstrate that the method is suitable for the determination of C18:1 DIOIC in human skin samples and transdermal perfusates