| Hair dye is a special kind of cosmetics. As a quite popular kind with consumers, oxidative hair dye is one of the most widely used type of hair dyes because of its better dyeing effect, longer time maintaining and so on. But the active ingredients in oxidative hair dyes are mostly aromatic amines and phenols, which are sensitive and easy to cause skin damage, and even cause cancer after your long time use. In view of the problem of safety in oxidative hair dyes, corresponding standards and regulations have been carried out to regulate the adding of these toxic and hazardous substances to oxidative hair dyes, and recommend the corresponding measurement method. Scientists are also actively seeking the best method to satisfy the increasing dye composition detection.This paper was carried out to research the detection method, which is focused on potentially harmful dyes to human health. In the selection of research objects,11representative aniline and phenol substances prohibited and restricted have been chosen, considering the cosmetics rules in China and UE, the existing detection methods and the add probability of dyes in samples; In the selection of detection methods, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was seleced. A method of simple, rapid and sensitive detection of11substances has been developed, through the optimization of sample pretreatment conditions and detection conditions of HPLC-MS/MS. The research contents and results of were as follows:In the study of pre-treatment of samples, ultrasonic assisted extraction technology was the main method, and have designed L9(34) orthogonal test and single-factor experiment to optimize the conditions, and the optimum pretreatment conditions were: the extraction solvent was5%methanol aqueous solution, the antioxidant was ascorbic acid and ultrasonic extraction for10minutes. In order to eliminate the influence of surface active substances in hair samples on the measurement of target components, the article selected the nonpolar n-hexane to extraction at the same time, and purificated through SPE C18column.In the study of the HPLC-MS/MS, this thesis examined the influence of the liquid chromatographic column, mobile phase, gradient elution program and MS/MS conditions on the separation and response value degree of11components, and finally selected the EC-C18column for separation, methanol-10mmol/L ammonium acetate aqueous solution as the mobile phase, and the multi-reaction monitoring scan mode (MRM) to collect mass spectrometric data, and realized multiple simultaneous determination of isomers in10minutes by electrospray ion source ESI (+)/(-) mode switching and the external standard method for quantification.The detection limits of this method were lower than9.43μg/g, the average recoveries ranged form87.8%to118.1%, and the relative standard deviations (RSD) were below than7.37%(n=6). So this analytical method is simple, rapid and sensitive.This method achieves effective extraction and separation of11substances prohibited and restricted in oxidative hair dye. It will not only contribute to the national testing organizations to supervise and manage the commercial samples, but also provide a useful attempt to analysis and detect the import and export of hair dye. |
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