臺灣博碩士論文加值系統

近年來食品安全相關的議題備受國人注意，相關多起茶葉農藥殘留超標事件新聞報導也層出不窮，本研究對飲用之茶葉是否含有殺蟲劑陶斯松(Chlorpyrifos)之農藥殘留(Pesticide Residues)進行檢測，先將Chlorpyrifos以質譜儀選定建立最佳母離子和子離子及碰撞能量，並建檔標準品層析滯留時間，於樣品前處理方式評估三種不同萃取溶媒：分別為Cyclohexane : 1-propanol (1:1 v/v)、Toluene : Chloroform (4:1 v/v)、以及Toxi-tubes® B，最後使用評估出來的最佳條件以氣相層析質譜儀(GC/MS)建立準確、簡單與快速分析法定性定量茶品中的農藥殘留。使用1L空白茶飲為基質配製100-2000 μg/mL 五種不同濃度檢量線標準溶液，經液液萃取後注入儀器分析，其檢量線範圍在100-2000 ng/mL 間呈現良好的線性關係，且精密度與準確度之同日內及異日間偏差，均在可接受範圍內(CV%<15%)，並評估平均萃取回收率(Recovery)、最低檢測極限(LOD)及最低定量極限(LOQ)。最後以完成之實驗方法，抽樣檢測市售茶葉、茶飲是否有農藥殘留並做統計分析，以期能建立農藥的快速檢測平台，將可對我國食品安全控管有實質性的助益。

In recent years, food safety topics have been valued by people. Many related reports also came out one after the others. The pesticide residue in tea potential health risks associated with exposure to detected pesticides. It should make people to attention. The aim of this study was the development, optimization, and validation of a simple, rapid, specific, and sensitive gas chromatography–mass spectrometry method for the determination of chlorpyrifos in tea. Evaluate three different types of extraction solvents, and we choose the best. The prepared samples were analysed with GC–MS in the selected ion monitoring mode (SIM) using one target and two qualitative ions for chlorpyrifos. After optimization and validation of liquid–liquid extraction, we use GC/MS multiple reaction monitoring (MRM) mode analyze samples. Prepare 1L tea as blank and make five different concentrates (50-1000ug/mL) as calibration curve. For validation of the technique, the following figures of merit were evaluated: accuracy, precision, calibration linearity and limits of detection and quantitation. This method was successfully incorporated into an overall analytical scheme, designed for the analysis of chlorpyrifos present in tea samples, and the study help government to sampling inspection of tea

中文摘要……………………………………………………………………………………..i
英文摘要……………………………………………………………………………………..ii
致謝…………………………………………………………………………………………..iv
目錄…………………………………………………………………………………………..vii
表目錄………………………………………………………………………………………..x
圖目錄…………………………………………………………………………………….….xi
第一章 緒論………………………………………………………………………………….1
1.1 前言......................................................................................................................1
1.1.1台灣茶葉的特質、種類與發展情況................................................................1
1.1.2台灣茶農使用的農藥概況................................................................................3
1.1.3研究動機............................................................................................................4
1.2 文獻回顧..............................................................................................................6
1.2.1農藥陶斯松的藥理特性及人體危害案例........................................................6
1.2.2常用農藥分析樣品前處理技術........................................................................8
1.2.3有關陶斯松分析的文獻探討............................................................................10
1.3 研究目的..............................................................................................................11
第二章 實驗材料與方法.........................................................................................................17
2.1 樣品來源..............................................................................................................17
2.2 藥品與試劑..........................................................................................................17
2.2.1藥物標準品/內標準品.......................................................................................17
2.2.2 化學試劑...........................................................................................................17
2.3 標準品與化學溶劑的配製..................................................................................18
2.3.1標準品溶液的配製......................................................................................18
2.3.2內標準品溶液的配製..................................................................................18
2.3.3化學試劑的配製..........................................................................................19
2.4實驗儀器設備與材料.....................................................................................19
2.4.1儀器設備......................................................................................................19
2.4.2材料...................................................... .......................................................19
2.5 儀器與分析設定條件....................................................................................20
2.5.1氣相層析質譜儀分析設定條件..................................................................20
2.5.2定性定量離子之選擇..................................................................................21
2.5.3定性方法設定................................................................... ..........................21
2.5.4定量方法設定......................................................... ........ ...........................21
2.6樣品前處理........................................................................... ........ ........ .......22
2.6.1萃取條件評估................................................................................ .............22
2.6.2三種萃取方法之實驗步驟..........................................................................22
2.7檢量線的建立......................................................................... ... .... ...............26
2.7.1校正曲線之實驗步驟.......................................................... ....... ................26
2.7.2校正曲線之測定.......................................................... ..... .. .......................26
2.8.分析方法確效........................................................................ ..... ...................27
2.8.1 準確度與精密度的評估.................................................................... .........27
2.8.2 偵測極限與定量極限的評估......................................................................27
2.8.3 回收率的評估.......................................................................... ...................28
2.8.4 基質效應的評估......................................................................... ................28
2.9 真實樣品農藥殘留之檢測............................................................... .............28
2.9.1 樣品定性實驗步驟.................................................. ...................................29
2.9.2 儀器檢測步驟.................................................. ............................................29
2.9.3 陶斯松定量實驗步驟...............................................................................29
第三章 結果與討論.........................................................................................................31
3.1 標準層析圖與質譜圖..................................................................................31
3.1.1 定性定量離子之選擇...............................................................................31
3.1.2滯留時間之確認........................................................................................32
3.2 最佳萃取條件評估......................................................................................35
3.3 校正曲線之結果評估..................................................................................37
3.4 準確度與精密度之結果評估......................................................................38
3.5 偵測極限與定量極限之結果評估...............................................................40
3.6 回收率之結果評估.......................................................................................40
3.7 基質效應之結果評估...................................................................................41
3.8 抽樣真實樣品之農藥殘留統計探討...........................................................44
第四章 結論......................................................................................................................46
參考文獻............................................................................................................................48

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