以固相微萃取法配合高效能液相層析儀偵測水中磺胺類抗生素

簡易檢索 / 詳目顯示

回結果列表

研究生：	陳淑樺
論文名稱：	以固相微萃取法配合高效能液相層析儀偵測水中磺胺類抗生素
指導教授：	黃賢達
口試委員:
學位類別：	碩士 Master
系所名稱：	理學院 - 化學系 Department of Chemistry
論文出版年：	2004
畢業學年度：	92
語文別：	中文
論文頁數：	78
中文關鍵詞：	固相微萃取法、磺胺類抗生素
相關次數：	點閱：4 下載：0
分享至:	分享至facebook 分享至twitter

查詢本校圖書館目錄查詢臺灣博碩士論文知識加值系統勘誤回報

本篇論文是以固相微萃取法結合高效能液相層析儀來偵測自然界水樣中的磺胺類抗生素，而實驗中所要分析的七種磺胺類抗生素分別為：sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamonomethoxine與sulfamethoxazole。
實驗中利用固相微萃取法(SPME)此種前處理方式來吸附水樣中的磺胺類抗生素，再經由SPME/HPLC的介面進入高效能液相層析儀中進行分離及定量。
本篇論文的研究重心在於探討各種實驗變因對固相微萃取效率所造成的影響，而需要探討的變因包含有纖維種類、萃取時間、浸泡時間、脫附時間、樣品攪拌速率、脫附液組成、樣品酸鹼值、夾帶、萃取溫度、離子強度及溶劑效應等十一種，在歸納了最理想的萃取條件後(纖維種類:CW/TPR;萃取步驟:萃取時間20分鐘、萃取溫度20℃、樣品攪拌速率850 rpm、樣品酸鹼值5.1、離子強度:添加20%的氯化鈉;脫附步驟:浸泡時間4分鐘、脫附時間1分鐘、脫附液組成:acetonitrile/water :18/82,移動相組成)，並將此偵測方法應用於真實樣品(客雅溪溪水)的分析。
由實驗結果發現，此分析方法的偵測極限可達趨近ng/ml的層級，且再現性高，線性相關係數(R2)在25~800 ng/ml的濃度範圍內介於0.986~0.999之間，而當其應用於溪水的分析時，回收率除了sulfacetamide由於本身的偵測訊號小又受到溪水基質干擾嚴重使得積分不易而偏低(52.1%)外，其餘六個待測物都達到不錯的結果(83.1〜96.6%)，可直接用簡單的檢量線法定量。

第一章    緒論..................................................................................................1
    1-1 前言.................................................................................................1
    1-2 磺胺類抗生素................................................................................2
    1-3 固相微萃取法................................................................................4
      1-3-1 直接固相微萃取(direct SPME)之原理..............................4
    1-4 磺胺類抗生素的檢測方法...........................................................7
第二章 實驗部分.........................................................................................10
    2-1 試藥................................................................................................10
    2-2 標準溶液和真實樣品...................................................................10
    2-3 儀器裝置........................................................................................11
    2-4 實驗步驟........................................................................................12
第三章 結果與討論.....................................................................................15
    3-1 各種影響變因探討.......................................................................15
       3-1-1 纖維的種類..........................................................................15
       3-1-2 萃取時間..............................................................................16
       3-1-3 脫附模式..............................................................................17
       3-1-4 浸泡的時間..........................................................................18
       3-1-5 脫附的時間..........................................................................18
      3-1-6 脫附液的組成......................................................................19
       3-1-7 攪拌速率..............................................................................20
       3-1-8 夾帶.......................................................................................20
       3-1-9 樣品溶液的pH值...............................................................21
       3-1-10 萃取溫度............................................................................22
       3-1-11 溶劑強度的影響...............................................................23
       3-1-12 離子強度的影響...............................................................24
    3-2 方法偵測極限、精密度和線性..................................................27
    3-3 環境樣品的測試...........................................................................28
第四章 結論..................................................................................................29
第五章 參考文獻.........................................................................................30

                                

(1) Chee-Sanford,J.C.;Aminov,R.I.;Krapac,I.J.;Garrigues-Jeanjean,N.;Mackie,R.I.“Occurrence and diversity of tetracycline resistance genes in lagoons and groundwater underlying two swine production facilities” Appl.Environ.Microbiol.2001,67,1494.
(2) Yang,S.;Carlson,K. “Evolution of antibiotic occurrence in a river through pristine, urban and agricultural landscapes ”Water Research2003,37,4645.
(3) Guardabassi,L.;Petersen,A.;Olsen,J.E.;Dalsgaard,A. “Antibiotic resistance in Acinetobacter spp. isolated from sewers receiving waste effluent from a hospital and a pharmaceutical plant ”Appl.Environ. Microbiol.1998,64,3499.
(4) Goni-Urriza,M.;Capdepuy,M.;Arpin,C.;Raymond,N.;Caumette,P.;Quentin,C.“Impact of an urban effluent on antibiotic resistance of riverine Enterobacteriaceae and Aeromonas spp.” Appl.Environ.Microbiol.2000,66,125.
(5) 陳德輝，常用的抗生素《第二版》，2003.
(6) 林誠一等，“磺胺噻唑餵飼土番鴨之探討”，畜產研究，1993，26(2)，155.
(7) Agarwal,V.K.“High-performance liquid chromatographic methods for the determination of sulfonamides in tissue, milk and eggs”J.Chromatogr.1992,624,411.
(8) Korpimäki,T.;Brockmann,E.-C.;Kuronen,O.;Saraste,M.;Lamminmäki,U.;Tuomola,M.“Engineering of a broad specificity antibody for simultaneous detection of 13 sulfonamides at the maximum residue level”J.Agric.Food Chem.2004,52,40.
(9) Hartig,C.;Storm,T.;Jekel,M. “Detection and identification of sulphonamide drugs in municipal waste water by liquid chromatography coupled with electrospray ionisation tandem mass spectrometry”J.Chromatogr.A1999,854,163.
(10) Hirsch,R.;Ternes,T.A.;Haberer,K.;Mehlich,A.;Ballwanz,F.;Kratz, K.-L. “Determination of antibiotics in different water compartments via liquid chromatography-electrospray tandem mass spectrometry”J.Chromatogr.A1998,815,213.
(11) Lindsey,M.E.;Meyer,M.;Thurman,E.M. “Analysis of trace levels of sulfonamide and tetracycline antimicrobials in groundwater and surface water using solid-phase extraction and liquid chromatography /mass spectrometry”Anal.Chem.2001,73,4640.
(12) Arthur,C.L.;Pawliszyn,J. “Solid phase microextraction with thermal desorption using fused silica optical fibers”Anal.Chem.1990,62,2145.
(13) Chen,J.;Pawliszyn,J.B. “Solid phase microextraction coupled to high-performance liquid chromatography” Anal.Chem.1995,67,2530.
(14) Salleh,S.H.;Saito,Y.;Kiso,Y.;Jinno,K. “Solventless sample preparation procedure for organophosphorus pesticides analysis using solid phase microextraction and on-line supercritical fluid extraction/high performance liquid chromatography technique”Anal.Chim.Acta2001,433,207.
(15) Boyd-Boland,A.A.;Pawliszyn,J. Solid-Phase Microextraction Coupled with High-Performance Liquid Chromatography for the Determination of Alkylphenol Ethoxylate Surfactants in Water”Anal.Chem.1996,68,1521.
(16) Wu,L.;Almirall,J.R.;Furton,K.G.“An improved interface for coupling solid-phase microextraction(SPME) to high performance liquid chromatography (HPLC) applied to the analysis of explosives”J.High.Resol.Chromatogr.1999,22,279.
(17) Negrao,M.R.;Alpendurada,M.F. “Solvent-free method for the determination of polynuclear aromatic hydrocarbons in waste water by solid-phase microextraction–high-performance liquid chromatography with photodiode-array detection ” J.Chromatogr.A,1998,823,211.
(18) Gbatu,T.P.;Sutton,K.L.;Caruso,J.A. “Development of new SPME fibers by sol–gel technology for SPME-HPLC determination of organometals” Anal.Chim.Acta1999,402,67.
(19) Jia,C.;Luo,Y.;Pawliszyn,J. “Solid phase microextraction combined with HPLC for determination of metal ions using crown ether as selective extracting reagent” J.Microcolumn.Sep.1998,10,167.
(20) Queiroz,M.E.C.;Silva,S.M.;Carvalho,D.;Lancas,F.M. “Solid-phase microextraction-liquid chromatography (SPME-LC) determination of lamotrigine simultaneously with carbamazepine and carbamazepine 10,11-epoxide in human plasma”J.Sep.Sci.2002,25,91.
(21) McCooeye,M.A.;Mester,Z.;Ells,B.;Barnett,D.A.;Purves,R.W.;
Guevremont,R. “Quantitation of amphetamine, methamphetamine, and their methylenedioxy derivatives in urine by solid-phase microextraction coupled with electrospray ionization-high-field asymmetric waveform ion mobility spectrometry-mass spectrometry”Anal.Chem.2002,74,3071.
(22) Lock,C.M.;Chen,L.;Volmer,D.A. “Rapid analysis of tetracycline antibiotics by combined solid phase microextraction/high performance liquid chromatography/mass spectrometry” Rapid.Commun.Mass.Spectrom.1999,13,1744.
(23)Bevill,R.F.;Schemske,K.M.;Luther,H.G.;Dzierzak,E.A.;Limpoka,M.;
Felt,D.R. “Determination of sulfonamides in swine plasma” J.Agric.Food Chem.1978,26,1201.
(24)Perkins,J.R.;Games,D.E.“Analysis of sulphonamides using supercritical fluid chromatography and supercritical fluid chromatography-mass spectrometry” J.Chromatogr.1991,540,239.
(25)Heifetz,C.L.;Chodubski,J.A.;Decarlo,M.O.;Fisher,M.W. “Disc-agar diffusion microbiological assay procedure for determining serum and urine levels of sulfacytine and other sulfonamides ”Appl.Microbiol.
1971,21,893.
(26)Muldoon,M.T.;Holtzapple,C.K.;Deshpande,S.S.;Beier,R.C.;Stanker,
L.H. “Development of a monoclonal antibody-based cELISA for the analysis of sulfadimethoxine.1.Development and characterization of monoclonal antibodies and molecular modeling studies of antibody recognition” J.Agric.Food Chem.2000,48,537.
(27)Koch,H.;Mooser,A.E. “Confirmatory method for sulfonamide residues in animal tissues by gas chromatography and pulsed positive ion-negative ion-chemical ionization mass spectrometry”J.AOAC Int.1993,76,976.
(28)Cannavan,A.;Hewitt,S.A.;Blanchflower,W.J.;Kennedy,D.G. “Gas chromatographic-mass spectrometric determination of sulfamethazine in animal tissues using a methyl/trimethylsilyl derivative”Analyst
1996,121,1457.
(29)Suhre,F.B.;Simpson,R.M.;Shafer,J.W. “Qualitative /quantitative determination of sulfamethazine in swine tissue by gas chromatographic/electron impact mass spectrometry using a stable isotope labeled internal standard” J.Agric.Food Chem.1981,29,
727.
(30)Tarbin,J.A.;Clarke,P.;Shearer,G. “Screening of sulphonamides in egg using gas chromatography-mass-selective detection and liquid chromatography-mass spectrometry” J.Chromatogr.B1999,729,127.
(31)Reeves,V.B. “Confirmation of multiple sulfonamides residues in bovine milk by gas chromatography-positive chemical ionization mass spectrometry” J.Chromatogr.B1999,723,127.
(32)Kao,Y.M.;Chang,M.H.;Cheng,C.C.;Chou,S.S.“Multiresidue determination of veterinary drugs in chicken and swine muscles by high performance liquid chromatography”Journal of Food and Drug Analysis2001,9,84.
(33)Heller,D.N.;Ngoh,M.A.;Donoghue,D.;Podhorniak,L.;Righter,H.;
Thomas,M.H. “Identification of incurred sulfonamide residues in eggs:methods for confirmation by liquid chromatography-tandem mass spectrometry and quantitation by liquid chromatography with ultraviolet detection” J.Chromatogr.B2002,774,39.
(34)Long,A.R.;Hsieh,L.C.;Malbrough,M.S.;Short,C.R.;Barker,S.A.“Multiresidue method for the determination of sulfonamides in pork tissue” J.Agric.Food Chem.1990,38,423.
(35)Cavaliere,C.;Curini,R.;Corcia,A.D.;Nazzari,M.;Samperi,R. “A simple and sensitive liquid chromatography-mass spectrometry confirmatory method for analyzing sulfonamide antibacterials in milk and egg” J.Agric.Food Chem.2003,51,558.
(36)Abián,J.;Churchwell,M.I.;Korfmacher,W.A. “High-performance liquid chromatography-thermospray mass spectrometry of ten sulfonamide antibiotics. Analysis in milk at the ppb level” J.Chromatogr. 1993,629,267.
(37)Kristiansen,G.K.;Brock,R.;Bojesen,G.“Comparison of flow injection/thermospray MS/MS and LC/thermospray MS/MS methods for determination of sulfonamides in meat and blood” Anal.Chem.1994,66,3253.
(38)Verzegnassi,L.;Savoy-Perroud,M.-C.;Stadler,R.H. “Application of liquid chromatography-electrospray ionization tandem mass spectrometry to the detection of 10 sulfonamides in honey” J.Chromatogr.A2002,977,77.
(39)Fuh,M.-R.S.;Chan,S.-A. “Quantitative determination of sulfonamide in meat by liquid chromatography-electrospray –mass spectrometry”Talanta2001,55,1127.
(40)Jen,J.-F.;Lee,H.-L.;Lee,B.-N. “Simultaneous determination of seven sulfonamide residues in swine wastewater by high-performance liquid chromatography” J.Chromatogr.A1998,793,378.
(41)Louch,D.;Motlagh,S.;Pawliszyn,J. “Dynamics of organic compound extraction from water using liquid-coated fused silica fibers” Anal.Chem.1992,64,1187.
(42)Berg,J.R. “Automation and optimization of solid-phase microextraction”Anal.Chem.1992,64,1960.
(43)Ai,J. “Solid phase microextraction for quantitative analysis in nonequilibrium situations” Anal.Chem.1997,69,1230.
(44)Górecki,T.;Pawliszyn,J. “Sample introduction approaches for solid phase microextraction/rapid GC” Anal.Chem.1995,67,3265.
(45)Djozan,D.;Assadi,Y.;Haddadi,S.H. “Anodized aluminum wire as a solid-phase microextraction fiber” Anal.Chem.2001,73,4054.
(46)Giardina,M.;Olesik,S.V. “Application of low-temperature glassy carbon films in solid-phase microextraction” Anal.Chem .2001,73,5841.
(47)Wu,J.;Pawliszyn,J. “Polypyrrole-coated capillary coupled to HPLC for in-tube solid-phase microextraction and analysis of aromatic compounds in aqueous samples” Anal.Chem.2001,73,55.
(48)The Merck index (12th)
(49)Prichard,E.;Mackay,G.M.;Points,J.Trace Analysis:A structured approach to obtaining reliable results1996,177.
(50)Scheppers,S.;Wercinski,A.Solid-phase microextraction-A Practical
Guide,Varian Chromatography System Walnut Creet,California 1999
,21.

全文公開日期本全文未授權公開 (校內網路)
全文公開日期本全文未授權公開 (校外網路)

簡易檢索 / 詳目顯示

相關論文