臺灣博碩士論文加值系統

摘要
本研究分別利用固相萃取連結高效能液相層析儀及微透析裝置連結高效能液相層析儀分析蜂蜜中十二種磺胺劑含量。實驗探討（1）以液相層析同時分析十二種磺胺劑之最佳化條件，（2）探討影響線上固相萃取之最佳化條件，包括：樣品注射量、樣品溶液pH值、樣品溶液加鹽的影響，和（3）微透析方面之最佳化條件，包括：灌注液流速和收集時間、樣品溶液pH值和灌注液極性修飾劑濃度的影響、鹽類效應。並以各別之最佳化條件探討固相萃取連結高效能液相層析儀及微透析裝置連結高效能液相層析儀的再現性、線性範圍及其偵測極限，及應用此二種技術於真實樣品中磺胺劑之檢測。
實驗結果，以逆相C18層析管柱，及動相流速1.0ml/min之甲酸/乙腈作梯度流析，偵測波長為270nm可以合理的分離十二種磺胺劑。線上固相萃取之最佳條件為注射量500μl及樣品溶液pH值=5.0。微透析之最佳條件為灌注液以40％乙腈、1.06μl/min之流速收集時間為15分鐘和樣品溶液pH=5.0。
以最佳實驗條件下分析標準添加十二種磺胺劑的蜂蜜，微透析裝置連結高效能液相層析儀方法各磺胺劑回收率分佈為52﹪~74﹪；偵測極限分佈為13~18ppb。固相萃取連結高效能液相層析儀方法各磺胺劑回收率分佈為56﹪~102﹪；偵測極限分佈為0.3~3ppb。

Abstract
The purpose of the study is to analyze 12 sulfonamides in honey by SPE on-line with HPLC and micro-dialysis on-line with HPLC. The study investigate（1）the optimal conditions of HPLC to simultaneous analyze 12 sulfonamides,（2）the optimal conditions of on-line SPE, including the sample injection volume, the pH, and the salt adding of the sample solution, and（3）the optimal conditions of on-line micro-dialysis, including the flow rate, collection time, pH, and modifier of perfusate as well as the salt adding effect of the sample. By the optimal conditions, the linear range, consistency, and detection limit were studied by both of the two on-line methods. And the real honey samples were examined by the proposed methods.
The optimal conditions of HPLC analysis is C18 reverse-phase column with the flow rate of 1.0 ml/min of gradient elution of formic acid aqueous solution/acetonitrile and the detection wavelength set at 270 nm. The optimal conditions of the On-line SPE analysis were 500μl of injection volume and the sample solution adjusted to pH5.0. The optimal conditions of the micro-dialysis were 40％ acetonitrile as perfusate with the flow rate of 1.06μl/min, 15min collection time, and the sample solution adjusted to pH5.0.
The honey sample spiked with 12 sulfonamides were investigated by the optimal conditions of the two on-line methods. The recoveries of were 52﹪~74﹪, and the detection limits were 13~18ppb of the 12 sulfonamides for micro-dialysis on-line with HPLC method. The recoveries of were 56﹪~102﹪, and the detection limits were 0.3~3ppb of the 12 sulfonamides for SPE on-line with HPLC method.

目 錄
摘要…………………………………………………………………………I
英文摘要…………………………………………………………………Ⅱ
圖次目錄………………………………………………………………Ⅲ
表次目錄…………………………………………………………………Ⅴ
簡語表…………………………………………………………………Ⅶ
第一章 緒論………………………………………………………………1
一、前言………………………………………………………‥………1
二、磺胺劑概述…………………………………………………………2
（一）磺胺劑的使用………………………………………………2
（二）磺胺劑的法規限制…………………………………………3
（三）磺胺劑的主要組成、結構及性質…………………………6
（四）磺胺劑的偵測方法…………………………………………6
三、微透析分析方法概述………………………………………………11
（一）微透析之理論介紹…………………………………………11
（二）透析薄膜的介紹……………………………………………14
（三）微透析技術應用與相關研究………………………………15
四、線上固相萃取（On-lin SPE）分析法概述………………………17
（一）固相萃取（SPE）之簡介……………………………………17
（二）關於線上固相萃取（On-line SPE）方法之介紹……………18
五、研究動機……………………………………………………‥……20
第二章 研究方法………………………………………………‥……21
一、實驗藥品、器材、儀器設備……………………………‥……‥21
（一）藥品……………………………………………‥………‥21
（二）器材…………………………………………………………23
（三）儀器設備……………………………………………‥……23
二、藥品配製……………………………………………………………26
（一）沖提液的配製………………………………………………26
（二）磺胺劑100ppm儲備溶液的配製…………………………26
（三）磺胺劑標準溶液的配製……………………………………27
（四）鹽析溶液的配製……………………………………………27
（五）真實樣品的配製……………………………………………28
三、實驗過程……………………………………………………………29
（一）實驗玻璃器皿矽烷化過程…………………………………29
（二）液相層析方法的建立………………………………………29
（三）透析薄膜的探討……………………………………………31
（四）微透析方法的建立…………………………………………33
（五）固相萃取管柱的探討………………………………………34
（六）線上固相萃取方法的建立…………………………………36
（七）真實樣品的分析……………………………………………38
第三章 結果與討論……………………………………………………39
一、液相層析方法的建立………………………………………………39
（一）UV偵測波長的選擇………………………………………39
（二）動相條件的選擇……………………………………………42
（三）管柱溫度……………………………………………………42
（四）梯度沖提……………………………………………………42
（五）液相層析方法再現性的測試………………………………43
（六）校正曲線建立及其偵測極限………………………………43
二、微透析分析方法的建立……………………………………………43
（一）透析流速和收集時間的探討………………………………50
（二）灌注液中有機修飾劑濃度的影響…………………………54
（三）鹽析效應的影響……………………………………………56
（四）微透析暨層析方法再現性的測試…………………………60
（五）校正曲線建立及其偵測極限………………………………60
（六）真實樣品的分析……………………………………………63
三、線上固相萃取分析方法的建立……………………………………63
（一）樣品注射量的探討…………………………………………63
（二）樣品溶液pH值的影響……………………………………68
（三）樣品溶液加鹽的影響………………………………………71
（四）線上固相萃取暨層析方法再現性的測試…………………76
（五）校正曲線建立及其偵測極限………………………………76
（六）真實樣品的分析……………………………………………81
第四章 結論……………………………………………………………86
參考文獻………………………………………………………………89

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