- 學位論文
發展微乳化電層析方法檢測環境水樣中的磺胺類藥物
Development of microemulsion electrokinetic chromatographic method for sulfonamide analyses in environmental water
摘要
本論文是以微乳化電層析(microemulsion electrokinetic chromatography, MEEKC)技術進行磺胺類藥物(sulfonamides)分離的研究，在尋找最好的分離條件後，為達到更好的偵測感度，進行線上樣品濃縮(on-line sample concentration)方法的開發。研究發現磺胺類藥物隨著溶液pH值轉變，可以陰離子、中性或陽離子存在，在低pH值條件下以陽離子選擇徹底注射 (cation-selective exhaustive injection and sweeping, CSEI-Sweeping) 方式放大磺胺類藥物的訊號效果不佳。接下來嘗試在較高pH值條件下，以陰離子選擇徹底注射(anion-selective exhaustive injection and sweeping, ASEI-Sweeping)方式進行其線上濃縮，效果明顯提升，但其中SPD分析物無法檢測到。最後結合陰離子選擇注射與陽離子選擇注射(anion-cation-selective exhaustive and sweeping, ACSEI-Sweeping)兩步驟進行線上濃縮，發現可以檢測所有磺胺類分析物，且其檢測感度接近單獨ASEI-Sweeping方式。 論文另一部分嘗試以反向遷移微胞堆積-陰離子注射(stacking with reversed migration micelles - anion selective exhanstive injection﹐SRMM-ASEI)方式進行磺胺類藥物線上濃縮。探討樣品基質pH值與電壓注射秒數等因素對於放大效果之影響。最後比較SRMM-ASEI與ACSEI-Sweeping兩種方法效果，並且討論應用於環境中水樣(地下水、魚塭水與養殖廢水)檢測磺胺類藥物的可行性。
並列摘要
In this thesis, sensitive and selective on-line concentration method coupled with microemulsion electrokinetic chromatography (MEEKC) technology has been mainly developed to detect and separate sulfonamide compounds. After optimal the separation condition, several on-line sample concentration methods were examined to find the better method for improving detection sensitivity of sulfonamides. All sulfonamides are able to be converted to anionic, neutral or cationic forms. A cation-selective exhaustive injection and sweeping (CSEI-sweeping) method was first used to enhance the sulfonamide signals under a sample matrix of low pH condition. The result indicated that it’s not good for sulfonamide concentration. Next, an anion-selective exhaustive injection and sweeping (ASEI-sweeping) method under a sample matrix of high pH was evaluated. The ASEI-sweeping method enhanced significantly their signals, but sulfapyridine (SPD) could not be detected. Consequently, a combination of ASEI- and CSEI-sweeping method (anion-cation-selective exhaustive and sweeping, ACSEI-sweeping) was utilized to stack the sulfonamides. All the sulfonamides could be detected by this ACSEI-sweeping method, and a relatively good detection sensitivity that was close to ASEI-sweeping method, was acquired. The other part of this thesis attempted to process the on-line sample concentration of sulfonamides by stacking with reversed migration micelles-anion selective exhaustive injection (SRMM-ASEI) method. The effect of sample matrix’s pH and electrokinetic injection time on the stacking ability of sulfonamides were examined. The concentration ability between the ACSEI-sweeping and SRMM-ASEI methods was also compared. Finally, the feasibility of the two on-line concentration methods that were applied to the determination of sulfonamides in environmental water sample (ground water and aquaculture water), was also evaluated.