| Due to the upcoming regulation of fragrance allergens in cosmetics, in this dissertation, a series of analytical procedures are studied for the routine analysis of 35 fragrances. Among these 35 compounds, 20 are believed to be the leading cause of allergic contact dermatitis and are found in cosmetic products. The remaining fragrance chemicals are banned from use in cosmetic products.; The separation step of the analytical process is effectively optimized with an aid of computer simulation software, DryLab. The reliability of resulting predictions is evaluated for conventional gas chromatography and Flash gas chromatography. Under both linear and multi-ramp temperature programs, retention time predictions are always excellent with correlation coefficient between predicted and experimental plots approaching 1.000 for all the studies performed here; the predictions of peak width at half height and resolution also show good agreement with experimental data for method development purposes.; Chromatographic software, DryLab, simplifies and speeds up the process of gas chromatographic method development. The improvements of instrumentation are also very important for saving time. The use of Flash gas chromatography reduces the analysis time dramatically by employing shorter lengths of capillary columns, higher carrier gas velocity and resistive heating.; Beside a gas chromatographic separation method, a reliable conventional GC-quadrupole MS detection method is also developed for the determination of 20 fragrance chemicals that are most frequently reported as contact allergens in perfume products. The data acquired in full-scan mode (SCAN) are used to identify the target suspect fragrance allergens in perfumes and the data obtained in the selected-ion acquisition mode (SIM) are used to get quantitation results.; With the present methodology, six commercially available perfumes are analyzed. According to the protocol of the European Union that the presence of individual suspect fragrance allergen has to be indicated in the list of ingredients when its concentration exceeds 10 ppm in leave-on products, the tested perfumes appear unsatisfactory. They all contain the target fragrance allergens, and the corresponding concentrations are all above 10 ppm. Due to the great composition complexity of perfumes, more work is needed to detect all target suspect fragrance allergens.; To extend the application of current detection method to analyze other cosmetics and household products with complex sample matrices, a simple, effective and solvent-free, fiber protective technique, headspace solid phase microextraction (HS-SPME), is introduced.; The selected HS-SPME conditions are effectively applied to simultaneously extract all 20 target fragrance allergens from a 10 ppm standard solution and six perfumes. Most SPME results compare favorably with direct injection results. However, linalool is detected as a possible candidate by the direct injection method; but it is positively identified by the SPME method. Additionally, to detect some of low concentration level of fragrance allergens (e.g. benzyl alcohol, citronellol and eugenol, etc.), the selected HS-SPME conditions need to be further optimized. Under the headspace mode, the application of current conditions can be easily extended to analyze a variety of cosmetic products.; In conclusion, a fast, reliable, qualitative and quantitative detection method that is suitable to analyze most cosmetic products in all quality control laboratories is successfully established. |
