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Microextraction technology development (3/4)- extraction method development for endocrine disrupting

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This project is to investigate the determination of 40 compounds including endocrine disrupting chemicals, antibiotic and cosmetic compounds in water by microextraction technique. Two methods including stir bar sorptive extraction (SBSE) and dispersive liquid–liquid microextraction (DLLME) were selected for evaluation and comparison. For the compounds of phthalate, SBSE method using PDMS type stir bar with 20% methanol in waters could have the best result. Recoveries ranged from 76% to 141%. The method detection limit could be down to ppt level (ng/L), so the blank of system was very important. It was difficult to remove contamination of DBP and DEHP in background as Marega, M. and Fankhauser-Noti, A. studies described. DLLME method with toluene and acetone were used as the extraction solvent and disperser solvent. Under the optimized conditions the enrichment factors for phthalate compounds were ranged from 176.6 to 299.7 folds. Average recoveries were the range of 68-116%. For the compounds of musk, SBSE method using PDMS type with the desorption temperature 300℃ and desorption time 10 mins. The recoveries were between 83% and 113%. The recoveries of DLLME were between 52% and 69%. The extraction efficiency of SBSE was better than that of DLLME. For the compounds of UV filter, there were residues of OMC, BP3 and EHS for SBSE method in the TDU-GC/MS system. The best recoveries were 54% ~ 212%. DLLME using cyclohexane as the extraction solvent with vortex technique, the recoveries were between 21% and 92%. For the compounds of antibiotic and pharmaceutical, SBSE method using EG-silicone type could have good extraction efficiency. The pH value of sample affects the recoveries. At pH 2, amoxicillin and ampicillin have the best extraction efficiency (recovery ranges between from 64% and 57%). Penicillin G, sulfadimethoxine, sulfamethazine, sulfamethoxazole, sulfamonomethoxine and tylosin have the best extraction efficiency at pH 4. The maximum recovery of 6 compounds was 85%. Using DLLME technology extract amoxicillin, ampicillin, chlortetracycline, oxytetracycline and tetracycline in water at pH 2 could have the best extraction efficiency. At pH 4, penicillin G, sulfadimethoxine, sulfamethazine, sulfamethoxazole, sulfamonomethoxine and tylosin could have the best extraction efficiency. Erythromycin could have the best extraction efficiency at pH 8, the recovery was 65%. The real samples taken from Er-ren River in Tainan, Cheng-ching lake and Tsao-kung channel in Kaohsiung. SBSE method was applied to the determination of 40 compounds in these samples. The recoveries of these compounds in real sample were similar to spiked in ultrapure water show these methods can be available for real samples.
Keyword
Stir bar sorption extraction (SBSE ),Dispersive liquid-liqud microextraction (DLLME),Endocrine disrupting chemicals,Antibiotic,Cosmetic compound
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