Determination of free formaldehyde in cosmetics by pre-column derivatization, extraction inhibition and high performance liquid chromatography

Abstract

Pre-column derivatization and inhibition by solvent extraction were applied to determine free formaldehyde in cosmetics by high performance liquid chromatography (HPLC). Due to the rapid decomposition of formaldehyde donors in the derivatization, it is hard to detect the amount of the free formaldehyde in cosmetics. The formaldehyde directly reacted with 2,4-dinitrophenylhydrazine in acetonitrile-phosphate buffer (pH 2) (1: 1, v / v) solution for 2 min, then dichloromethane extraction was used to induce the decomposition of formaldehyde donors. The extract was diluted with acetonitrile and then determined by HPLC. The formaldehyde derivative was separated on an Agilent C18 column (250 mm ×4. 6 mm, 5 μm) at 30 °C with acetonitrilewater (60:40, v / v) as mobile phase at a flow rate of 1. 0 mL / min, and detected at the wavelength of 355 nm. The recoveries were from 81% to 106% at the spiked levels of 50, 100, 500, 1 000 μg / g of formaldehyde in shampoo, milk, cream, hand cleaner, toothpaste, nail polish, powder separately, and the relative standard deviations (n =6) were less than 5. 0%. The limit of quantification of the formaldehyde in cosmetics was 50 μg / g. The method has been applied to the determination of free formaldehyde in real samples and the results showed that the release by formaldehyde donors was inhibited. The method has the advantages of simple operation, good accuracy and meets the requirement of determination of free formaldehyde in cosmetics.