| Synthetic musks are believed to have the same fragrance as natural musk and used in a wide variety of daily use. For the harmfulness of synthetic musks and their agglomeration in organism, the content of synthetic musks in products is limited in many countries. To such a situation, it put forward higher requirements for the analysis detection technology of synthetic musks. Synthetic musks entry into the environment with the discharge of sanitary sewage, it is the key link for them enters the organism by concentration in soil and sediment for their lipophilic performance. In this paper, a novel nano-sorbent is presented. The pretreatment method of the sample has improved, and the analysis for the simultaneous determination of 7 synthetic musks in soil and sediment by gas chromatography-mass spectrometry (GC-MS) has been established. There are two research parts in this paper:(1) The reverse-phase emulsion system constituted by CTAB, hexyl alcohol, hexane and aqueous solution was utilized to synthesize Zn-Al layered double hydroxide (Zn-Al LDHs) and Mg-Al layered double hydroxide (Mg-Al LDHs). The external factors like the water/surfactant molar ratio (?) and ammonium hydroxide concentration impact on the LDHs were investigated, and the layered double oxide (LDO) was calcined with above LDH which was prepared by reversed-phase microemulsion method forms the flower-like texture with large surface area. When the concentration of ammonia hydroxide increased from 1 molˇL-1 to 3 molˇL-1, supersaturation is increase leading to surface content decrease, and by changing the value of ? can control the morphology of LDH. The results showed that the special microstructure has still retained after calcination and it obtained more specific surface for LDO which has calcined by LDHs.(2) The experiment compared the adsorption performance of above four kinds of materials (Zn-Al LDHs, Zn-Al LDO, Mg-Al LDHs, Mg-Al LDO) and silica gel for 7 synthetic musks (musk ambrette, musk tibetene, musk moskene, musk ketone, musk xylene, phantolide, and tonalide). Finally, Zn-Al LDO which is in place of conventional silica gel was used as SPE to concentrate and cleanup synthetic musks in sediment. In this study, a method was established for the determination of 7 synthetic musks in sediment by Zn-Al LDO as SPE column coupled with GC-MS. Extraction times of ultrasonic and mechanical shaking, extraction solution, and elution volume were optimized. In this study,7 synthetic musks are successfully extracted by a mixture solution of N-hexane and acetone from 2.0g sediment, and separated and purified by Zn-Al LDO SPE column. The results indicated that this method has a satisfactory linearity ranged from 10 ngˇmL-1 to 1000 ngˇmL-1. The recoveries and the limits of detections (LODs) using this method are ranged from 93.7-105.2%(n=3) and 0.11-0.79 ngˇmL-1, respectively. And in all case, the relative standard deviation was lower than 7.80%(n=3,5). This method is simple and accurate, which has been successfully applied to determine synthetic musks in soils and sediments.In this work, LDO were calcined from LDHs which were synthesized by reversed-phase microemulsion method and were used as sorbent in SPE for the determination of 7 synthetics musks in soils and sediments. It exhibits satisfying capacity of separation and purification, and the new SPE column packing can be reuse by calcined at high temperature to reduce test cost. |
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