Determination of N-nitrosodiethanolamine in cosmetic products by headspace solid phase microextraction using a novel aluminum hydroxide grafted fused silica fiber followed by gas chromatography-mass spectrometry analysis

Abstract

A method based on headspace solid phase microextraction with a new fiber, coupled with gas chromatography-mass spectrometry was developed for the determination of NDELA in cosmetic samples. The fiber provides Lewis acid-base interaction between its surface and analyte functional groups. The fiber was prepared by grafting aluminum tri-tert-butoxide on the surface of a fused silica. The optimization of SPME conditions showed that NDELA can be most effectively extracted at 70°C, in 15 min, with a sample volume of 0.5 (Vs/Vt), stirring rate of 150 rpm, desorption time of 5 min, desorption temperature of 260°C and at 12.5% (w/w) concentration of NaCl. Under the optimized conditions, LOD of 1 μg Kg(-1) and a calibration curve with correlation coefficients greater than 0.9897 and a linearity range from 6 to 10000 μg Kg(-1) were obtained. The intra-day and inter-day precision and accuracy were evaluated at four concentration levels. All of the values for accuracy and precision were lower than the acceptable limit of 15%. The fiber to fiber repeatability was 8.7%. The method was applied for the analysis of real samples including hair shampoo, body shampoo, dishwashing liquid and hand washing liquid. Relative recoveries were achieved in the range of 95-99%.