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

• Published in: Talanta (Oxford) 2013-02, Vol.105, p.347-353
• Main Authors: Davarani, Saied Saeed Hosseiny, Masoomi, Leila, Banitaba, Mohammad Hossein, Zhad, Hamid Reza Lotfi Zadeh, Sadeghi, Omid, Samiei, Azam
• Format: Article
• Language: English
• Subjects: Aluminum Hydroxide - chemistry; Aluminum hydroxide grafting; Cosmetic; Cosmetics; Cosmetics - chemistry; Desorption; Diethylnitrosamine - analogs & derivatives; Diethylnitrosamine - chemistry; Fibers; Gas Chromatography-Mass Spectrometry - methods; Gas chromatography–mass spectrometry; Grafting; Headspace solid phase microextraction; Liquids; N-nitrosodiethanolamine (NDELA); Solid Phase Microextraction - methods; Solid phases; Spectrometry; Spectroscopy
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2012.10.053

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 15min, with a sample volume of 0.5 (Vs/Vt), stirring rate of 150rpm, desorption time of 5min, desorption temperature of 260°C and at 12.5% (w/w) concentration of NaCl. Under the optimized conditions, LOD of 1μgKg−1 and a calibration curve with correlation coefficients greater than 0.9897 and a linearity range from 6 to 10000μgKg−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%. ► We introduce a new SPME fiber preparation method based on aluminum grafting process. ► Grafted Al-fused silica was applied for extraction of NDELA from cosmetic products. ► Al provides acidic sites which can effectively interact with basic sites of NDELA. ► The method is more simple, fast and efficient than other developed methods.