6533b7d6fe1ef96bd1265d66

RESEARCH PRODUCT

Determination of free formaldehyde in cosmetics containing formaldehyde-releasing preservatives by reversed-phase dispersive liquid-liquid microextraction and liquid chromatography with post-column derivatization.

Alberto ChisvertAmparo SalvadorPablo MirallesM. José AlonsoSandra Hernandorena

subject

AcetonitrilesLiquid Phase Microextraction02 engineering and technologyCosmetics01 natural sciencesBiochemistryChemistry Techniques AnalyticalAnalytical Chemistrychemistry.chemical_compoundLimit of DetectionFormaldehydeAcetonitrileDerivatizationDetection limitChromatographyElution010401 analytical chemistryOrganic ChemistryExtraction (chemistry)Preservatives PharmaceuticalReproducibility of ResultsWaterGeneral Medicine021001 nanoscience & nanotechnology0104 chemical sciencesSolventchemistryReagentSolvents0210 nano-technologyEnrichment factorChromatography LiquidToluene

description

Abstract An analytical method for the determination of traces of formaldehyde in cosmetic products containing formaldehyde-releasing preservatives has been developed. The method is based on reversed-phase dispersive liquid–liquid microextraction (RP-DLLME), that allows the extraction of highly polar compounds, followed by liquid chromatography–ultraviolet/visible (LC–UV/vis) determination with post-column derivatization. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the selected conditions, a mixture of 500 μL of acetonitrile (disperser solvent) and 50 μL of water (extraction solvent) was rapidly injected into 5 mL of toluene sample solution. The extracts were injected into the LC–UV/vis system using phosphate buffer 6 mmol L−1 at pH 2 as mobile phase. After chromatographic separation, the eluate merged with a flow stream of pentane-2,4-dione in ammonium acetate solution as derivatizing reagent and passed throughout a post-column reactor at 85 °C in order to derivatize formaldehyde into 3,5-diacetyl-1,4-dihydrolutidine, according to Hantzsch reaction, which was finally measured spectrophotometrically at 407 nm. The method was successfully validated showing good linearity, an enrichment factor of 86 ± 2, limits of detection and quantification of 0.7 and 2.3 ng mL−1, respectively, and good repeatability (RSD

10.1016/j.chroma.2018.02.031https://pubmed.ncbi.nlm.nih.gov/29478830