Determination of additives in cosmetics by supercritical fluid extraction on-line headspace solid-phase microextraction combined with gas chromatography-mass spectrometry.
ABSTRACT A new hyphenated technique couples supercritical fluid extraction in situ derivatization and on-line headspace solid-phase microextraction to gas chromatography-mass spectrometry (SFE in situ derivatization on-line HS-SPME-GC-MS) for the determination of paraben preservatives and polyphenolic antioxidants in cosmetics. The preservatives and antioxidants were extracted from the cosmetic matrices with supercritical carbon dioxide at a pressure of 13,840 kPa. The supercritical fluid extraction was performed at 55 degrees C for 10 min of static extraction then 15 min of dynamic extraction. The extractant subsequently was derivatized in situ with the silylation reagent N,O-bis(trimethylsilyl)trifluoroacetamide with 0.1% trimethylchlorosilane. The product was then adsorbed on a polyacrylate solid-phase microextraction (SPME) fiber in the headspace. Sea sand was used as a dispersive material in the SFE step. The analytical linear ranges for the preservatives and antioxidants were found to be from 10 to 1000 ng g(-1) with RSD values below 7.8%. The detection limits ranged from 0.5 to 8.3 ng g(-1). These results are better than those obtained by using only SPME or SFE for trace preservatives and antioxidants analysis in cosmetic matrices. The new method was successfully utilized to determine the amounts of preservatives and antioxidants in real cosmetics without the need for tedious pretreatments.
Article: Optimization and Validation of RP-HPLC-UV/Vis Method for Determination Phenolic Compounds in Several Personal Care Products.[show abstract] [hide abstract]
ABSTRACT: An HPLC method with ultraviolet-visible spectrophotometry detection has been optimized and validated for the simultaneous determination of phenolic compounds, such as butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) as antioxidants, and octyl methyl cinnamate (OMC) as UVB-filter in several personal care products. The dynamic range was between 1 to 250 mg/L with relative standard deviation less than 0.25% (n = 4). Limits of detection for BHA, BHT, and OMC were 0.196, 0.170, and 0.478 mg/L, respectively. While limits of quantification for BHA, BHT, and OMC were 0.593, 0.515, and 1.448 mg/L, respectively. The recovery for BHA, BHT, and OMC was ranged from 92.1-105.9%, 83.2-108.9%, and 87.3-103.7%, respectively. The concentration ranges of BHA, BHT, and OMC in 12 commercial personal care samples were 0.13-4.85, 0.16-2.30, and 0.12-65.5 mg/g, respectively. The concentrations of phenolic compounds in these personal care samples were below than maximum allowable concentration in personal care formulation, that is, 0.0004-10 mg/g, 0.002-5 mg/g, and up to 100 mg/g for BHA, BHT, and OMC, respectively.International Journal of Analytical Chemistry 01/2011; 2011:858153.