| 研究生: |
陳鑫昌 Hsin-Chang Chen |
|---|---|
| 論文名稱: |
利用毛細管電泳結合線上濃縮方法分離奈磺酸鹽之機制探討 Analysis of naphthalenesulfonate compounds by cyclodextrin-mediated capillary electrophoresis with sample stacking |
| 指導教授: |
丁望賢
Wang-Hsien Ding |
| 口試委員: | |
| 學位類別: |
碩士 Master |
| 系所名稱: |
理學院 - 化學學系 Department of Chemistry |
| 畢業學年度: | 91 |
| 語文別: | 中文 |
| 論文頁數: | 80 |
| 中文關鍵詞: | 樣品堆積 、環糊精 、奈磺酸鹽 、毛細管電泳 |
| 外文關鍵詞: | sample stacking, capillary electrophoresis, cyclodextrin, naphthalenesulfonate |
| 相關次數: | 點閱:15 下載:0 |
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本研究主要是建立樣品線上濃縮技術(on-line concentration)以提高毛細管電泳(CE)的靈敏度。毛細管電泳是近年來相當受到重視的分析技術,但往往受限於毛細管的光徑長度,使得在以UV的偵測上,無法有效降低分析的偵測極限。利用樣品線上濃縮技術來提高靈敏度的方式,不必更改或更換任何儀器設備,以達到簡便且經濟的需求。其原理是增加毛細管中樣品的進樣量,以不同方式將樣品聚集濃縮,提高樣品的相對濃度。
奈磺酸鹽類(Naphthalene Sulfonates)是指磺酸根取代基在奈丸的不同位置上取代所形成之位置異構物,在製藥與化學工業的產品製造上均被廣泛使用。由於這類化合物具有很高的水溶性與穩定性,易隨水流四處擴散,加上廢水處理無法適當降解這類化合物,以致這些物質隨廢水排放入自然水環境中,進而污染水源及影響環境生態。此外由於一般的毛細管區帶電泳(CZE)並無法有效分離位置異構物,因此將利用毛細管環糊精修飾區帶電泳對位置異構物進行分析,以達有效分離。
研究中將改良反向電極極性堆積模式(Reverse Electrode Polarity Stacking Mode、REPSM),對樣品進行堆積進而分離,並改變緩衝溶液中b-、g-環糊精之組成成份及比例,以求分離達到最佳化。在最佳的樣品堆積分離條件下,方法偵測極限可達到4mg/L。遷移時間與波峰的再現性也因加入內標準品而有顯著的改善,此分析物的定性與定量更加精密。此方法亦成功應用至飲用水之微量分析。
This study systematically investigates the optimal conditions for analyzing the positional isomers of multi-charged naphthalenesulfonate compounds by cyclodextrin-mediated capillary electrophoresis (CE). Specifically, this work employs large-volume sample injection with the electrode polarity switching technique. The most effective separation and sample stacking conditions was 15 mM borate buffer with a mixture of b- and g-cyclodextrin (CD) (concentration ratio 3:7 mM) at pH 9.2 and 25℃, and the sample hydrodynamic injection of up to 60 seconds at 3 psi (around 1802 nL). Significant selective and sensitive improvements were observed and a more than 100-fold enrichment was achieved (based on peak area). The reproducibility of migration time and quantitative results of stacking CE can be improved by using internal standards. The quantitation limits of these naphthalenesulfonate isomers, based on a signal-to-noise (S/N) ratio above 10, can be reached about 4 mg/L with UV detection. This method was successfully applied to determine the trace amount of naphthalenesulfonate isomers in a spiked drinking water sample.
** 王榮德,常見的環境病與職業病診斷方法,中華民國環境職業醫學會會訊,第1期,第4- 12頁,民國83年。
** 王榮樂,邁向21世紀的染色工業,染化雜誌,第180期,第28-32頁,民國88年。
** 染整顧問服務中心,紡織品生態與毒物監測的分析技術(2),染化雜誌,第175期,
第47-59頁,民國88年。
** 陳家祥,推動環保的染料和藥劑,染化雜誌,第183期,第29-37頁,民國88年。
** 陸德培,張滂,環糊精,中國大百科化學卷,第480頁,民國77年。
** 張文譚,不污染水環境的染色廢排水處理,染化雜誌,第175期,第10-13頁,
民國88年。
** 楊宗穎,以微胞電動力層析法對氯三環口井中性物種分離及線上濃縮研究,碩士論文,
國立台灣大學化學研究所,民國88年。
** 劉啟宏,芳香族磺酸鹽類有機污染物在水環境中的分析與研究,碩士論文,
國立中央大學化學研究所,民國90年。
** http://www.CEandCEC.com
** Alonso, M.C., Castillo, M., Barcelo, D., Solid phase extraction of polar
benzene and naphthalenesulfonates in industrial effluents followed by
unequivocal determination with ion-pair chromatography/electrospray-mass
spectrometry, Anal. Chem. 71 (1999) 2586-2593.
** Altenbach, B., Giger, W., Determination of Benzene- and Naphthalene-
sulfonates in Wastewater by Solid-Phase Extraction with Graphitized Carbon
Black and Ion-Pair Liquid Chromatography with UV Detection, Anal. Chem. 67
(1995) 2325-2333.
** Baker, D.R., Capillary Electrophoresis, John Wiley & Sons, Inc., 1995.
** Brilon, C., Beckmann, W., Appl. Enviorn. Microbiol. 42 (1982) 44.
** Brouwer, E.R., Tol, T.M., Lingeman, H., Brinkman, U.A.Th., Quim. Anal., 12
(1993) 88.
** Chien, R.L., Burgi, D.S., Field amplified sample injection in high
performance capillary electrophoresis, J. Chromatogr. 559 (1991) 141-152.
** Fanali, S., Enantioselective determination by capillary electrophoresis with
cyclodextrins as chiral selectors, J. Chromatogr. A 875 (2000) 89-122.
** Fischer, J., Jandera, P., Stanek, V., Effects of the working electrolyte
(cyclodextrin type and pH) on the separation of aromatic sulphonic acids by
capillary zone electrophoresis, J. Chromatogr. A 772 (1997) 385-396.
** Foret F., Krivankova L. and Bocek P., Capillary Zone Electrophoresis P8VCH,
Weiheim, 1993.
** Heinig, K., Vogt, C., Werner, G., Determination of linear
alkylbenzenesulfonates in industrial and environmental samples by capillary
electrophoresis, Analyst 123 (1998) 349-353.
** Khaledi, M.G., High Performance Capillary Electrophoresis: Theory,
Techniques, and Applications, John Wiley & Sons, Inc., 1998.
** Kok, S.J., Isberg, I.C.K., Gooijer, C., Brinkman, U.A.T., Velthorst, N.H.,
Ultraviolet laser-induced fluorescence detection strategies in capillary
electrophoresis: determination of naphthalene sulphonates in river water,
Anal. Chim. Acta 360 (1998) 109-118.
** Kuhn, R. and Hoffstetter-Kuhn, S., Capillary Electrophoresis: Principles and
Practices, Springer-Verlag, New York, 1993.
** Liu, C.H. and Ding, W.H., Analysis of linear alkylbenzene -sulfonates by
capillary zone electrophoresis with large volume sample stacking, J.
Chromatogr. A 929 (2001a) 143-150.
** Liu, C.H. and Ding, W.H., Determination of naphthalenesulfonic acid isomers
by large-volume on-line derivatization and gas chromatography-mass
spectrometry, J. Chromatogr. A 926 (2001b) 341-346.
** Liu, Z., Sam, P., Sirimanne, S.R., McClure, P.C., Field-amplified sample
stacking in micellar electrokinetic chromatography for on-column sample
concentration of neutral molecules, J. Chromatogr. A 673 (1994) 125-132.
** Loos, R., Niessner, R., Analysis of aromatic sulfonates in water by solid-
phase extraction and capillary electrophoresis, J. Chromatogr. A 822 ( 1998)
291-303.
** Luong, J.H.T., Nguyen, A.L., Achiral selectivity in cyclodextrin-modified
capillary electrophoresis, J. Chromatogr. A 792 (1997) 431-444.
** Monnig, C.A. Kennedy, R.T., Capillary Electrophoresis, Anal. Chem. 66 (1994)
280R-314R.
** Quirino, J.P., Terabe, S., On-line concentration of neutral analytes for
micellar electrokinetic chromatography. Ⅱ. Reversed electrode polarity
stacking mode, J. Chromatogr. A 791 (1997) 255-268.
** Quirino, J.P., Terabe, S., On-line concentration of neutral analytes for
micellar electrokinetic chromatography. 3. stacking with reverse migrating
micelles, Anal. Chem. 70 (1998a) 149-157.
** Quirino, J.P., Terabe, S., On-line concentration of neutral analytes for
micellar electrokinetic chromatography: IV. Field-enhanced sample injection,
J. Chromatogr. A 798 (1998b) 251-257.
** Quirino, J.P., Terabe, S., On-Line concentration of neutral analytes for
micellar electrokinetic chromatography. 5. Field-enhanced sample injection
with reverse migrating micelles, Anal. Chem. 70 (1998c) 1893-1901.
** Quirino, J.P., Terabe, S., On-line concentration of neutral analytes for
micellar electrokinetic chromatography: VI. Stacking using reverse migrating
micelles and a water plug, J. Chromatogr. B 714 (1998d) 29-38.
** Quirino, J.P., Terabe, S., Exceeding 5000-fold concentration of dilute
analytes in the micellar electrokinetic chromatography, Science 282 (1998e)
465-468.
** Reemtsma, T., Methods of analysis of polar aromatic sulfonates from aquatic
environments, J. Chromatogr. A 733 (1996) 473-489.
** Riediker, S., Ruckstuhl, S., Suter, M.J.F., Cook, A.M., Giger, W., p-
Toluenesulfonate in Landfill Leachates: Leachability from Foundry Sands and
Aerobic Biodegradation, Environ. Sci. Technol. 34 (2000) 2156-2161.
** Riediker, S., Suter, M.J.F., Giger, W., Benzene- and naphthalene-sulfonates
in leachates and plumes of landfills, Wat. Res. 34 (2000), 2069-2079.
** Shintani, H. Polonsky J. (eds.), Handbook of Capillary Electrophoresis
Application, Blackie Academic. London, 1997.
** Storm, T., Reemtsma, T., Jekel, M., Use of volatile amines as ion-pairing
agents for the high performance liquid chromatographic -tandem mass
spectrometric determination of aromatic sulfonates in industrial wastewater,
J. Chromatogr. A 854 (1999) 175-186.
** Terabe, S., Miyashita, S., Shibata, O., Barnhart, E.R., Alexander, L.R.,
Patterson, D.G., Karger, B.L., Hosoya, K., Tanaka, N., Separation of Highly
Hydrophobic Compounds by Cyclodextrin- Modified Micellar Electrokinetic
Chromatography, J. of Chromatogr. 516 (1990) 23-31.
** Wittich, R.M., Rast, H.G., Knackmuss, H.J., Degradation of naphthalene-2, 6-
and naphthalene-1, 6-disulfonic acid by a Moraxella sp., Appl. Enviorn.
Microbiol. 54 (1988) 1842-1847.
** Yoshinaga, M., Tanaka, M., Effect of urea addition on chiral separation of
dansylamino acids by capillary zone electrophoresis with cyclodextrins, J.
Chromatogr. A 710 (1995) 331-337.
** Zerbinati, O., Diana, I., Baiocchi, C., Trace naphthalene-sulfonates
determination in natural water sample, Intern. J. Environ. Anal. Chem. 74
(1999) 43-54.
** Zerbinati, O., Trotta, F., Giovannoli, C., Optimization of the cyclodextrin-
assisted capillary electrophoresis separation of the enantiomers of
phenoxyacid herbicides, J. Chromatogr. A 875 (2000) 423-430.
** Zerbinati, O., Vincenti, M., Pittavino, S., Gennaro, M.C., Fate of aromatic
sulfonates in fluvial environment, Chemosphere 35 (1997) 2295-2305.
** Zurrer, D., Cook, A.M., Leisinger, T., Microbial desulfonation of
substituted naphthalenesulfonic acids and benzenesulfonic acids, Appl.
Enviorn. Microbiol. 53 (1987) 1459-1463.