Study Of The Analytical Method For The Determination Of Synthetic Musks In Environment

Synthetic musks, as cheap substitutes for natural musks, are widely used in many personal care products, such as perfume, cream, body lotion, shampoo, soap, laundry soap powder etc. After production and use, synthetic musks may enter the wastewater system and be distributed widely in environment. Synthetic musks were detected in water, sludge, fish, shrimp, mussel and other aquatic animals, and even in people's adipose tissue, blood and breast milk and they are considered ubiquitous, persistent, bioaccumulative and toxic. Consequently much attention was paid to the potential hazardous of synthetic musks in recent years. The MX and MK, for example, were included in the prohibition on certain hazardous substances in consumer products (POHs) by Norwegian pollution control authority.Analysis and detection of synthetic musk in environment (such as water, soil, sediment, animals and plants) is crucial important for the monitoring those compounds in the distribution, transmission, transfer, and final degradation. In this paper, 8 kinds of synthetic musks (Cashmeran (DPMI), Celestolide (ADBI), Phantolide (AHDI), Traseolide (ATII), Galaxolide (HHCB), Tonalide (AHTN), Musk xylene (MX) and Musk ketone (MK)) were selected as the investigated subjects due to their wide applications. And rapid analysis and detection methods were established for various environmental matrices, specific research include the following:1. In this study, the method of ultrasound-assisted emulsification–microextraction (USAEME) coupled with gas chromatography mass spectrometry (GC/MS) was employed to detect 8 kinds of synthetic musk in aqueous solutions. 50μL chlorobenzene was used as extraction solvent, ultrasonic 5min, then centrifugate 5min at 4000rpm, the organic phase was for GC/MS analysis directly. The results showed the good linearities between analytic signal and analyte concentration in the range of 1-80ng/mL. The limits of detection were ranged from 0.003 to 0.005 ng/mL, and the recoveries for spiked samples were in the range of 96.2—102.9% with RSD between 2.3%—4.1%. Using this method, 15 water samples from Taihu Lake were detected. The results reflect the synthetic musks are distributed widely in lake; HHCB and AHTN are the main pollutants of synthetic musks compounds.2. In this study, a new extraction procedure, based on the accelerated solvent extraction (ASE) and in cell clean-up technique was developed and successfully coupled with gas chromatography-mass spectrometry (GC/MS) for the analysis of musks in sediment samples. An optimum experimental condition, solvent: n-hexane /acetone (1:1, V:V), extraction temperature: 100℃, 5min extraction time and 2 extraction cycles was obtained. The purification process was operated by in cell clean-up with Florisil. With this method, the limits of detection as low as 0.03-0.05ng/g, the recovery rate of 86.0%-104% and the RSD between 0.5—6.9% are achieved. When compared with soxhlet extraction (SE) and ultrasonic extraction (USE), ASE not only has the best extraction efficiency but also has advantages in extraction time and solvent consumption. Eight synthetic musks were evaluated in 15 sediment samples collected from 15 selected locations of Taihu lake. The results reflect current status of fragrance compounds pollution in this area, and provide basic data for environmental policy making. 3. In this paper, a new analytical method, based on the accelerated solvent extraction (ASE), in cell clean-up technique and gas chromatography/mass spectrometry (GC/MS), was developed for the determination of synthetic musks in aquatic products. The experiment conditions were initially optimized and the best extraction efficiency was obtained when n-hexane was used as the extraction solvent, the neutral aluminum oxide as the selective adsorbent and the temperature of extraction was set at 100℃. The limits of detection as low as 0.1-0.5 ng/g with linear range between 1-80 ng/g were achieved for eight synthetic musks. The recoveries for spiked samples were in the range of 85.3%—94.6% with RSD between 2.3%—8.4%. Using this method, the contents of 8 synthetic musks in 20 aquatic products of the Taihu lake were determined. The results show that the method is suitable for detection of synthetic musk in aquatic products.4. In this paper, a dye-sensitized photodegradation method was studied as a possible approach for the removal of synthetic musks. Four musks, i.e., Galaxolide (HHCB), Tonalide (AHTN), musk xylene (MX) and musk ketone (MK) were employed as the model compounds. Several important factors that may affect the degradation process were investigated in detail, these include the type of sensitizers and their concentrations, the pH and the temperature of reaction medium, and the initial concentration of synthetic musks. At the optimum conditions, the degradation rates of 84.6 %, 86.1%, 87.2 % and 49.2 % were achieved respectively for HHCB, AHTN, MX and MK in 60 min of visible light irradiation. The degradation processes were found to follow a pseudo first-order kinetics for all the musks. It was also found that the degradation rates in nature water were higher than that in pure water, suggesting that the dye-sensitized photodegradation method should be applicable to remove the synthetic musks from the wastewater.