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研究生:邱梅欣
研究生(外文):Mei-Hsin Chiu
論文名稱:多元性可拋棄式網版印刷電極分析技術平台之建立與應用
論文名稱(外文):The development of multiple analytical techniques coupled with disposable screen-printed electrodes
指導教授:曾志明曾志明引用關係
學位類別:博士
校院名稱:國立中興大學
系所名稱:化學系所
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:中文
論文頁數:127
中文關鍵詞:網版印刷電極抗生素高效能液相層析法電化學發光法
外文關鍵詞:screen-printed electrodeAntibioticsHPLCECL
相關次數:
  • 被引用被引用:3
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  • 收藏至我的研究室書目清單書目收藏:1
電化學分析系統最大的優點莫過於儀器價格相對便宜,且易於與其他分析系統連結,可彌補電化學分析方法之不足,使偵測系統更趨完善並增廣其應用性。本研究即以電化學偵測器所具有的操作簡單、價格低、與其他系統結合性高之特點為基礎,利用網版印刷電極高可變性、低交互污染等優點,延伸、發展多種偵測技術與分析方法。
本論文於第一、二章節內詳細介紹研究中所使用之碳、銀兩種工作電極與偵測的分析方法。第三章第一節闡述以網版印刷碳電極(Screen-printed carbon electrode, SPCE)為工作電極,利用電化學偵測器與電化學發光法之結合分別建立草酸與胺基配醣體抗生素的檢測。草酸測定分析法為光與電兩種偵測技術之結合,可於同一時間獲得電流訊號與光強度相關訊息,此一特點不僅有效增加線性範圍量級,且對於定量分析物更具雙重確認的功效。除此之外,利用電化學發光法特殊反應機構,可選擇性偵測具有二級胺結構的胺基配醣體抗生素。第二節中同樣以SPCE為工作電極,利用安培法結合流動注入分析系統(Flow Injection Analysis, FIA)進行青黴素類抗生素–Amoxicillin之偵測定。藉由MnO2反應器將Amoxicillin氧化(—ø–OH → —ø=O),所得產物可由電化學分析法於0.0 V (vs. Ag/AgCl)直接測得還原訊號,如此將大幅減少其他物種可能造成的干擾現象。此方法具有高選擇性、高靈敏度,無須藉由分離技術即可於複雜樣品中進行Amoxicillin定性與定量工作。
第四章,利用預氧化網版印刷碳電極(SPCE*)進行Lincomycin抗生素測定。SPCE*對Lincomycin的檢測具有降低偵測電位、提高偵測訊號之功效。此外本研究中亦與固相萃取法、高效能液相層析分離技術結合,並應用於飼料、鮮奶、蜂蜜、尿液等真實樣品測定。
第五章,利用銀網版印刷電極為發展的研究可分:銀網版印刷試片(Screen-Printed Silver Electrode Strip, SP-AgES) 與銀網版印刷單電極(Screen-Printed Silver electrode, AgSPE)兩種型式。第一節中利用SP-AgES結合線性掃描伏安法進行氯、溴、碘三種鹵素離子分析測定。藉由改善SP-AgES中參考電極的穩定性,可避免一般電化學偵測系統中常用Ag/AgCl (3 M KCl)參考電極存在著氯離子滲漏的風險,進而造成定量樣品中氯離子濃度的困難。第二節以AgSPE為工作電極進行汞重金屬偵測。利用AgSPE於偵測碘離子的高靈敏度與碘、汞離子反應後生成錯合物之化學原理,建構一套具有高選擇性偵測汞重金屬的分析方法,並將之應用於市售美容商品與環境水樣測定。
總而言之,本論文研究以造價低、操作簡便之電化學偵測系統為基礎,利用各類型網版印刷電極,結合多種不同學門與技術,發展多元化分析方法,並成功應用於各式真實樣品之鑑定與檢測。
Nowadays electroanalysis combined with other analytical work systems are well known for its broad application. In this doctoral thesis work, variety of electrochemical detectors developed with simple, low cost, easy useable screen-printed carbon electrodes and then applied for a spectrum of analysis.
The first two chapters explain the fabrication of different types of electrodes and brief introduction of techniques used in this research work. Section I of Chapter III explains the use of screen-printed carbon electrode, SPCE as a working electrode in the development of an electrochemical detector for the assay of aminoglycoside antibiotics. Determination of oxalic acid by the combination of electrochemiluminescence and electroanalysis techniques are also studied with simultaneous analysis of current and light intensity response and this technique not only effective in increasing the order of magnitude but also good for complex quantitative analysis with efficacy. While in Section II, SPCE working electrode combined with amperometric flow injection analysis used for analysis of penicillin type antibiotics; amoxicillin with MnO2 reactor. It is based on the well-known chemical conversion of catechols to o-quinones by MnO2 that can be subsequently easily determined by electrochemical reduction at inexpensive screen-printed carbon electrodes
Chapter IV deals with the use of preanodized screen printed carbon electrode (SPCE *) for the determination of lincomycin. Detection of lincomycin with a lower detection potential to enhance the effect of signal detection is achieved with SPCE*. The proposed electrochemical sensor is then coupled with techniques like solid-phase extraction and high-performance liquid chromatography for the further analysis of lincomycin in real samples such as feed, milk, honey, and urine.
The uses of two types of screen printed silver electrodes are extensively studied in chapter V. One type of electrode consists of an electrode strip with silver as working electrode, AgSPE and another one with the combination of all 3 electrodes with silver as working, counter and reference electrodes in a single strip, SP-AgES. The use of SP-AgES with combination of linear sweep voltammetry explored for halide ion determination (Cl-, Br-, and I-). SP-AgES with stable reference electrode can avoid the general electrochemical disadvantage while using Ag / AgCl (3 M KCl) reference electrode such as the risk of leakage of chloride ions during the quantitative analysis of halide ions. AgSPE is used for the determination of heavy metal like mercury (Hg) in the presence of potassium iodide. And this approach was further utilized to analyze hidden Hg in the cosmetic samples. Real sample assays were consistent with that of result obtained from ICP-OES, which confirm the applicability of the proposed method for practical application.
Overall in this doctoral research thesis a low cost and easy useable electrochemical detection system based on different types of screen printing electrodes combined with different analytical techniques are successfully applied for identification and detection of biologically and environmentally important sample of interest.
論文摘要 I
Abstract III
第一章 緒論 1
第一節 前言 1
第二節 各類型網版印刷電極介紹 3
第三節 電化學分析方法簡介 4
一、 循環伏安法 (Cyclic Voltammetry, CV) 4
二、 安培法 (Amperometric) 5
第四節 固相萃取(Solid Phase Extraction, SPE)原理簡介 7
第二章 儀器與藥品 8
第一節 儀器設備 8
第二節 藥品目錄與配製方法 10
一、 網版印刷碳電極結合多樣化偵測系統方法開發與建立 10
二、 預氧化網版印刷碳電極於藥物偵測之應用 10
三、 網版印刷銀電極開發與應用 11
第三章 網版印刷碳電極結合多樣化偵測系統方法的開發與建立 12
前言 12
第一節 電化學發光分析系統 13
一、 光與電同步分析系統進行草酸測定之研究 16
1-1 Ru(bpy)32+—C2O42–系統ELC反應機制與電化學行為探討 18
1-2 Ru(bpy)32+—C2O42–結合FIA系統之參數最佳化探討 21
1-2-2流速與Amperometric—ECL偵測系統之關係 22
1-3 Amperometric—ECL偵測系統之校正曲線建立 24
1-4 Amperometric—ECL偵測系統穩定性探討 26
1-5 結論 27
二、 利用CV—ECL系統選擇性偵測胺基配醣體抗生素 28
1-1 胺基配醣體抗生素電化學行為與ECL反應機制 31
1-2 CV–ECL偵測系統裝置簡介 35
1-3 CV–ECL偵測系統參數最佳化 36
1-3-1 掃描速度與ECL訊號關係 36
1-3-2 pH值與ECL訊號關係 37
1-4 檢量線之建立與系統穩定性測試 38
1-5 真實樣品測定 41
1-6 結論 42
第二節MnO2反應系統測定抗生素Amoxicillin 43
1-1 Amoxicillin電化學行為探討 45
1-2 物種結構與電化學行為關係 47
1-3 反應機制推導 48
1-4 系統參數最佳化 51
1-4-1 pH值效應探討 51
1-4-2 FIA系統—電位、流速探討 52
1-5 校正曲線與系統穩定性探討 54
1-6 MnO2—Amoxicillin 偵測系統之選擇性探討 56
1-7 真實樣品測定與應用 57
1-8 結論 59
1-9 未來展望 60
1-9-1 利用MnO2反應器結合UV–EC系統同步偵測Amoxicillin 60
1-9-2 利用MnO2反應器選擇性偵測胺基酸—Tyrosine 62
第四章 預氧化網版印刷碳電極於藥物偵測之應 70
前言 70
第一節 食品中Lincomycin殘留量測定 71
1-1 Lincomycin電化學行為探討 73
1-2 建立分析系統最佳化參數 75
1-2-1 預氧化條件探討 75
1-2-2 pH值效應探討 76
1-2-3 FIA 系統—電位探討 77
1-3 固相萃取樣品前處理 78
1-4 高效能液相層析法(HPLC)結合電化學偵測器分析系統 80
1-4-1 Lincomycin於有機溶劑下之電化學行為 81
1-4-2 HPLC系統—流動相的選擇 82
1-4-3 HPLC系統—校正曲線與穩定性 83
1-4-4 HPLC系統—真實樣品測定 84
1-5 結論 89
第二節 未來展望 90
第五章 銀網版印刷電極的開發與應用 94
前言 94
第一節 陰離子與銀網版印刷電極之電化學行為探討與偵測 96
一、 CV System—分析物之電化學行為探討 98
1-1 FIA System—各種陰離子之測定 101
1-1 參考電極穩定性探討 105
1-2 鹵素離子檢測 106
1-3 鹵素離子真實樣品測定 108
1-4 結論 110
第二節 汞重金屬偵測 111
一、 汞重金屬之測定—LSV System 113
1-1 SPCE與AgSPE電極比較 113
1-2 校正曲線與再現性 115
1-3 真實樣品測定 116
二、 汞重金屬之測定—FIA System 118
1-1 AgSPE結合安培法偵測碘離子 118
1-2 檢量線之建立 120
1-3 干擾測試 121
1-4 真實樣品測定 122
1-5 結論 123
第三節 未來展望 124
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