EPA-104-E3S4-02-01

104

1,780 千元

2015/02/26

2015/12/31

林維炤

環檢所

鄧名志

嘉南藥理大學

環境監測及檢測

攪拌子吸附萃取，分散式液液微萃取，內分泌干擾物、抗生素、 化妝品化合物

Stir bar sorption extraction (SBSE )，Dispersive liquid-liqud microextraction (DLLME)，Endocrine disrupting chemicals，Antibiotic，Cosmetic compound

葉錦芬

林維炤

(06)-2664911# 2401

radical891025@gmail.com

本計畫針對水中之內分泌干擾物、抗生素及化妝品化合物開發攪拌子吸附萃取（SBSE）與分散液液微萃取(DLLME)等2種微萃取技術，評估40項塑化劑類、麝香類、抗生素類及防曬劑類等化合物之濃縮效能及可行性。 塑化劑類化合物部分，以PDMS型攪拌子配合水樣中加入20%甲醇進行SBSE萃取效率佳，回收率76% ~ 141%，因測定濃度可低至ng/L，故實驗室環境中背景測定與空白樣品顯得相當重要，然而本研究經一連串處理模式仍難將DBP和DEHP背景干擾去除，Marega, M.與Fankhauser-Noti, A.等人的研究亦被此困擾；而DLLME則是以甲苯為萃取溶劑及丙酮為分散劑有良好萃取效率，其濃縮因子為176.6~299.7，回收率68% ~116%。 人工麝香類化合物部分，以PDMS型攪拌子進行SBSE萃取，脫附溫度提高至300℃及脫附時間維持10分鐘，其回收率85%~113%。以甲苯進行DLLME，回收率52% ~69%，整體評估，SBSE技術比DLLME技術適合萃取人工麝香待測物。 防曬劑類化合物部分，以SBSE分析在TDU-GC/MS系統內易有OMC、BP-3與EHS殘留，最佳回收率54%~212%；DLLME以環己烷為萃取溶劑搭配渦漩輔助方式有較佳的萃取效率，其回收率21% ~92%。 抗生素及藥劑類化合物部分，分析物本身之Ko/w (皆小於4且有負值) ，EG-silicone攪拌子對於大部分的抗生素及藥劑類均有不錯的萃取效果，而本研究待測物之回收率會受到pH值的影響，在pH 2環境下安莫西林及安匹西林有較好的萃取效率(回收率為64%與57%)，在pH 4環境下則是盤尼西林G、磺胺二甲氧嘧啶、磺胺二甲嘧啶、磺胺甲噁唑、磺胺一甲氧嘧啶及泰黴素有較好的萃取效率，最高回收率為85%；以DLLME技術萃取測試，在pH 2環境下安莫西林、安匹西林、氯四環黴素、羥四環黴素及四環黴素有較好的萃取效率; 而pH 4環境下則是盤尼西林G、磺胺二甲氧嘧啶、磺胺二甲嘧啶、磺胺甲噁唑、磺胺一甲氧嘧啶及泰黴素有較好的萃取效率；紅黴素則是在pH 8有較好的萃取效率，回收率為65%。 本計畫選擇SBSE方式進行真實樣品評估。真實樣品來源於台南二仁溪、高雄澄清湖、高雄曹公圳。結果顯示本研究待測物在真實水樣的添加回收率相似於在超純水的添加回收率，故此方法可適用於真實樣品之測定。

攪拌子吸附萃取，分散式液液微萃取，內分泌干擾物、抗生素、 化妝品化合物

EPA-104-E3S4-02-01.pdf

5MB

2016/2/1 上午 12:00:00

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.

Stir bar sorption extraction (SBSE )，Dispersive liquid-liqud microextraction (DLLME)，Endocrine disrupting chemicals，Antibiotic，Cosmetic compound