Research On Labelling Investigation And Detection Method Of 29 Fragrance Ingredients In Cosmetics

Along with the continuous development and progress of fragrance industry, fragrances have played a more and more important role in people’s daily life. Fragrances can bring people pleasant feeling, meanwhile there has been an increased emphasis on their safety issues. Related policies and regulations were consequently issued to restrict and constraint the use of fragrances in various countries.The labelling of 29 fragrance ingredients was investigated in cosmetics of three major categories including 970 samples in this study. A GC/MS method was established to detect 27 synthetic fragrance ingredients in cosmetics and perfume raw materials and then was applied for analyzing practical samples. Finally, the result consistency was discussed between label investigation and analysis. Additionally, the detection methods of oak moss extract and tree moss extract were preliminarily explored. The main conclusions obtained in this paper were as follows:1. According to the Cosmetic Classification (GB/T 18670-2002),970 cosmetic samples were classified and 29 fragrance ingredients were investigated. Statistical results showed that except for 6-methyl coumarin, musk xylene and musk ketone, one or more ingredients among the 26 fragrance ingredients with sensitization risk were found in 222 cosmetic samples according to their labels. The total labelling rate was 22.9%. For the cleanser, skin/hair care and make-up products, the labelling rates were 16.9%,20.1% and 31.5% respectively, which differed significantly. Besides, there was a significant difference in the labelling of different fragrance ingredients. The highest was linalool up to 87.4% and the amyl cinnamyl alcohol and tree moss extract were only 0.4%. Furthermore,16 samples labelled one fragrance ingredient,206 samples labelled two or more, the highest labelled 22 kinds, which suggested different fragrances were often simultaneously used to achieve a better effect.2. A GC/MS method was established for detection of 27 synthetic fragrances in cosmetics and perfume raw materials. Methanol was selected as extraction solvent and weak polar capillary column and El ion source were used for GC/MS analysis. The linear ranges of hydroxyisohexyl-3-cyclohexene carboxaldehyde, hydroxycitronellal and musk xylene were 5mg/L～50mg/L,5mg/L～50mg/L and 0.4mg/L-4mg/L in the method, respectively. Quantitative limits were 50mg/kg,50 mg/kg and4 mg/kg, respectively. The linear ranges were lmg/L～50mg/L for the rest of the 24 fragrances with the quantitative limits of 10mg/kg. All the correlation coefficients were greater than or equal to 0.996. Except for musk xylene, the spiked recovery rates of 26 fragrances ranged from 81.5% to 118% and the RSDs were lower than 10%, which suggested method characteristics met the requirements of routine analysis. The recovery rates of musk xylene ranged from 73.3% to 76.1%, for the possible reason was the use of low concentration and volatile fragrance as standard, which resulted in a less spiked amount than the theoretical value after pre-treatment.3. One or more fragrance ingredients among the 26 synthetic fragrance ingredients (except for 6-methyl coumarin) were detected in 40 cosmetics whose labels showed they contained fragrances and 29 perfume raw materials. The content ranged from 0.001% to 32.2%. The analytical results were basically consistent with label investigation.4. A method was explored for detecting 2 natural fragrances (oak moss extract and tree moss extract), which respectively separated 55 and 30 compounds. Active ingredients and their content may be different with various preparation processes because of the complexity of nature fragrances. Meanwhile, Lichen substances have almost the same characteristic components. So there were a lot of difficulties in the qualitative and quantitative analysis of this kind of natural fragrances. In this method, the relative contents were detected by the normalization method of peak area. By selecting methyl β-orcinolcarboxylate and methyl haematommate as the characteristic qualitative indicators for oak moss extract and methyl dihydroabietate as the characteristic qualitative indicators for tree moss extract. According to the practical sample test results, it was estimated that one perfume sample may contain oak moss extract whose content was about 0.06%, one perfume sample and two perfume raw materials may contain tree moss extract with the content of perfume was about 0.1% and of perfume raw materials was about 10%. The results matched with the label investigation.