臺灣博碩士論文加值系統

飼料中添加抗生素，使動物順利成長並抵抗疾病。如果禽畜生病時業者使用高劑量抗生素治療疾病，又沒遵守停藥期限制等情況，是肉品與蛋品殘留動物用藥的因素。本研究分析市售加工蛋品中5種磺胺劑磺胺嘧啶(Sulfadiazine, SDZ)、磺胺二甲基嘧啶(Sulfamethazine, SMT)、磺胺一甲氧嘧啶(Sulfamonomethoxine, SMM)、磺胺奎寧（Sulfaquinoxaline, SQX）、磺胺二甲氧嘧啶(Sulfadimethoxine, SDM）殘留情形。
加工蛋品均質後，以不同溶劑進行萃取研究，再以固相萃取法使樣品待測物部分純化及濃縮。本研究使用極致效能液相層析串聯質譜儀 UPLC/MS/MS 分析，其斷裂離子碎片SDZ 251.04>156.0, 251.04>92.1；SMT 279.16>124.0, 279.16>92.0；SMM 281.10>156.0, 281.10>92.0；SQX 301.10>155.9, 301.10>92.0及SDM 311.11>156.0, 311.11>92.0。線性範圍為 1 ppb ~ 100 ppb，校正曲線相關係數SDZ, R2 = 0.9985; SMT, R2 = 0.9993; SMM, R2 = 0.9999; SQX, R2 = 0.9983; SDM, R2 = 0.9998. 方法偵測極限 (MDL) SDZ: 1.95 ppb; SMT: 1.34 ppb; SMM: 1.83 ppb; SQX: 2.04 ppb; SDM: 1.85 ppb。

By feeding animals with antibiotics, the poultries can be raised with good health. However, if the industry used high-dose of antibiotics for the treatment of disease and did not comply with any governmental regulations of meat and egg, drug residues would be occurred in food. In this study, five different kinds of processed eggs obtained in the markets were used to analyze the sulfa drugs residues.
After the processed egg homogenizing, different organic solvents were used to study the extraction efficiency. The extracts were partially purified by solid-phase extraction. The ultra performance liquid chromatography tandem mass spectrometry UPLC/MS/MS was used to study five different sulfa drugs in this studies, and the fragments SDZ 251.04>156.0, 251.04>92.1；SMT 279.16>124.0, 279.16>92.0；SMM 281.10>156.0, 281.10>92.0；SQX 301.10>155.9, 301.10>92.0及SDM 311.11>156.0, 311.11>92.0 were used to mass analysis.The results shown the linear range of 1 ppb ~ 100 ppb could be achieved, correlation coefficient of SDZ, R2 = 0.9985; SMT, R2 = 0.9993;SMM, R2 = 0.9999; SQX, R2 = 0.9983; SDM, R2 = 0.9998. Method detection limit (MDL) SDZ: 1.95 ppb; SMT: 1.34 ppb; SMM: 1.83 ppb; SQX: 2.04 ppb; SDM: 1.85 ppb.

中文摘要………………………………………..………..……….……….I
英文摘要………………………………..………………..…….……….…Π

第一章、 前言...........................................................................................1
第二章、 文獻整理..................................................................................4
一、 磺胺劑的歷史沿革.………………………………...…………..….4
二、 磺胺劑的一般特性及抗菌機制…………………….…………......4
三、 磺胺劑的臨床應用………………………….…………………......5
四、 磺胺劑的副作用…………...…………………………..............…..6
五、 磺胺劑的法令規範……………………………………..……….....7
六、 磺胺劑的檢測方法……………………………………….…….….8
七、 磺胺劑萃取方法…………………………………………...…..…..9
八、 固相萃取（Solid Phase Extraction, SPE）…………….……….…10
九、 液相層析串聯質譜儀UPLC/MS/MS……………………….....…11
第三章、 實驗設備、材料與研究方法…………………………...…..13
一、 設備及材料………………………….………………...……….…13
二、 試藥及溶液配製…………………….……………..….….………15
1. 試藥………………………….…….…………..………...………15
2. 溶液配製………………………..……………..………....……...15
(1) 標準品配製……………………………….…………..……...…...16
(2) 內部標準品配製…………………………………………….....…16
(3) 檢量線配製……………………………………...………...…...…16
(4) 萃取溶液 Extraction solution C….................................................17
(5) 萃取溶液 Extraction solution D.....................................................17
(6) 移動相配製.....................................................................................17
(7) 0.5M HCl.........................................................................................17
(8) 5%Methanol....................................................................................17
(9) 20% Methanol.................................................................................17
(10) 90：10 Methanol：200mM Ammonium bicarbonatev(v/v).........17
(11) 3:7, ACN:H2O(v/v)........................................................................18
三、 研究方法………………………………...............…………..……18
1. 萃取液之選用……………....…………...…...................................18
2. 吸附劑之選用……………………….......……….................…......19
3. 萃取步驟(Extraction steps)…………………….….............….…...20
4. 淨化步驟(Purification steps)………………….............……….…..20
5. 收集樣品(Collection of samples)…………….............……...…….21
6. UPLC層析條件……………………………….............……….…..21
7. MASS分析條件………………………………….…................…..21
8. 方法偵測極限Method Detection Limite(MDL)……….................22
9. 樣品最終檢測濃度計算公式..........................................................24
第四章、 結果與討論...............................................................................25
一、 檢量線配製...................................................................................25
二、 預估方法偵測極限(Method Detectio Limit, MDL)……….........25
三、 方法偵測極限(Method Detectio Limit, MDL).............................25
四、 質譜儀分析條件...........................................................................26
五、 萃取液之比較...............................................................................26
六、 添加5種吸附劑，改善回收率之比較..........................................27
七、 添加回收率分析試驗...................................................................27
八、 逆向離子交換之固相萃取...........................................................28
九、 真實樣品之測定...........................................................................28
十、 法規值比較...................................................................................29
第五章、 結論............................................................................................30
第六章、 參考文獻....................................................................................32

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