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研究生:董雅華
研究生(外文):Yu-Hun Tung
論文名稱:以C4矽烷鍵合相為材質之固相萃取裝置連結高效能液相層析儀分析雞蛋中十四種磺胺劑含量
指導教授:楊慶成楊慶成引用關係
學位類別:碩士
校院名稱:國立高雄師範大學
系所名稱:化學系
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:2005
畢業學年度:93
語文別:中文
中文關鍵詞:磺胺劑
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摘 要
本研究擬開發以C4矽烷鍵合相為材質之固相萃取裝置連結高效能液相層析儀分析方法來檢測雞蛋中十四種磺胺劑。實驗探討,線上固相萃取連結高效能液相層析儀分析方法之最佳化條件,包括有動相和層析管柱的選擇、溫度、樣品pH值及注射量等因素。
實驗發現,線上固相萃取之最佳條件為注射量800μl及樣品溶液調整pH值為5;HPLC系統之最佳條件為使用C18逆相層析管柱、動相流速1.0ml/min之甲酸/乙腈作梯度流析及偵測波長設定在270nm,以此最佳化條件探討其線性範圍、相關係數及偵測極限(L.O.D.)。
將此方法之最佳化條件應用於真實雞蛋樣品的分析,發現雞蛋樣品中的十四種磺胺劑回收率分佈在72.3~109.7%。因此,本研究發展出利用線上固相萃取連結HPLC的精確快速分析方法,以檢測市售雞蛋中磺胺劑的含量。
Abstract
The purpose of the study is to develop a method for determining fourteen sulfonamide residues in eggs by C4 solid-phase extraction (SPE) with high performance liquid chromatography (HPLC). The study investigated the optimal condition of on-line SPE with HPLC, including the mobile phase, the stationary phase, temperature, pH value and injection volumn of sample .
It is found that the optimal conditions are 800μl of injection volumn, the sample solution adjusted to pH 5 for SPE and C18 reverse-phase column with the flow rate of 1.0 ml/min of gradient elution of formic acid aqueous solution∕acetonitrile , the detection wavelength set at 270 nm for HPLC analysis. By the optimal conditions, the linear range, r2 and the limits of detection were studied .
Applying the developed method to analyze the real egg samples by the optimal condition, it is found that the recoveries of 14 sulfonamides in eggs are ranged from 72.3 to 109.7%. Therefore, a rapid method for determination of fourteen sulfonamides in commercial eggs using on-line SPE with HPLC has developed .
第一章 緒論----------------------------------------------------------1
一、前言-------------------------------------------------------------1
二、磺胺劑的介紹------------------------------------------------------2
三、線上固相萃取(On-line SPE)分析方法的介紹---------------------------15
四、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
二、藥品配製---------------------------------------------------------27
三、實驗過程---------------------------------------------------------30
四、真實樣品的分析----------------------------------------------------37
第三章 結果與討論----------------------------------------------------40
一、液相層析方法的建立------------------------------------------------40
二、線上固相萃取分析方法的建立-----------------------------------------47
三、真實樣品的分析----------------------------------------------------67
第四章 結論---------------------------------------------------------82
第五章 參考文獻-----------------------------------------------------84
第五章 參考文獻
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