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研究生:李宜真
研究生(外文):yi-chen Lee
論文名稱:利用GC/MS進行茶葉中殘留農藥Carbofuran的最佳化含量分析方法研究
論文名稱(外文):The optimization of GC/MS-based analysis method for the content of residual pesticides Carbofuran in tea samples
指導教授:蘇昭瑾
指導教授(外文):Chaochin Su
口試委員:王修璇李文仁
口試日期:2018-07-13
學位類別:碩士
校院名稱:國立臺北科技大學
系所名稱:分子科學與工程系有機高分子碩士班
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2018
畢業學年度:106
語文別:中文
論文頁數:40
中文關鍵詞:食品安全茶飲農藥殘留內標準品氣相層析質譜分析法定性分析定量分析ChlorpyrifosMethomylCarbofuran-d3Carbofuran
外文關鍵詞:Internal standardsGC/MSLC/MSQualitative analysisQuantitative analysisChlorpyrifosMethomylCarbofuran-d3Carbofuran
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Carbofuran(加保扶)是氨基甲酸鹽類農藥,它的化學式為 C12H15NO3。目前市面上毒性最強的農藥之一。外觀為無色固體結晶,介質是火山的灰粒,溶濕性好,遇露水便能溶解進到土壤中,發揮其殺蟲的作用。殺蟲範圍廣,兼具防治地上、地下害蟲、根蟎及線蟲,又可混合肥料拌土使用,省錢又省工。
隨著消費意識抬頭,社會大眾對於食品安全越來越重視,如麵包香料、牛肉、塑化劑、餿水油、毒奶粉事件、市售飲料方面(如農藥量超標)等,都是民眾關心的課題。
本研究主要在於使用GC/MS萃取茶飲中殘留農藥Carbofuran,先選用最適用之萃取方式。再來測試最適用之內標準品【Carbofuran-d3、Methomyl、Chlorpyrifos】去評估分析那一種內標準品做出的結果較為GC/MS儀器最佳分析條件。使用最適用之分析內標準品做方法確效,評估日間變動、日內變動及萃取回收率,利用基質效應評估實驗的可行性,最後使用評估出來的最佳條件來盲測試市售茶飲是否有農藥Carbofuran殘留。
Carbofuran is a carbamate pesticide with a chemical formula of C12H15NO3. One of the most toxic pesticides on the market. The appearance is colorless solid crystal, the medium is volcanic ash particles, and the solubility is good. When exposed to water, it can be dissolved into the soil to play an insecticidal effect. It has a wide range of insecticides, and it can prevent and control above-ground and underground pests, root mites and nematodes, and can also be mixed with fertilizers for soil use, saving money and labor.
With the rise of consumer awareness, the public is paying more and more attention to food safety, such as bread spices, beef, plasticizers, swill oil, tainted milk powder incidents, and commercial beverages (such as excessive pesticides). Question.
This study mainly uses GC/MS to extract the residual pesticide Carbofuran in tea, first select the most suitable extraction method (such as liquid phase liquid extraction or commercially available Toxi-tubeB). Then test the most suitable internal standards [Carbofuran-d3, Methomyl, Chlorpyrifos] to evaluate and analyze the results of the internal standard compared to the best analytical conditions for GC/MS instruments. The test results are evaluated and validated using the most applicable analytical standards. The daytime variation, intraday variation and extraction recovery rate are evaluated, the feasibility of the experiment is evaluated using the matrix effect, and the best conditions evaluated are used. Come to blindly test whether the commercial tea has a residue of Carbofuran pesticide.
目 錄

中文摘要.....................................................................................................................................i
英文摘要....................................................................................................................................ii
致謝...........................................................................................................................................iv
目錄..........................................................................................................................................vii
表目錄........................................................................................................................................ix
圖目錄........................................................................................................................................x
第一章 緒論...............................................................................................................................1
1.1前言.........................................................................................................................1
1.2農藥加保扶的簡介、作用及人體危害.................................................................3
1.3有關加保扶分析的文獻探討.................................................................................5
1.4研究目的.................................................................................................................6
第二章 實驗方法.....................................................................................................................11
2.1農藥標準品/內標準品、材料、試劑與樣品.......................................................11
2.1.1標準品/內標準品.........................................................................................11
2.1.2材料..............................................................................................................11
2.1.3試劑..............................................................................................................11
2.1.4樣品..............................................................................................................12
2.2標準品/內標準品的配製......................................................................................12
2.2.1樣品溶液配製..............................................................................................12
2.2.2內標準品溶液配製......................................................................................12
2.3實驗使用之設備器材...........................................................................................13
2.4樣品的前處理.......................................................................................................13
2.5實驗步驟...............................................................................................................13
2.5.1樣品定性實驗步驟........................................................................................13
2.5.2儀器檢測步驟................................................................................................13
2.5.3農藥定性實驗步驟........................................................................................14
2.5.4農藥定量實驗步驟........................................................................................14
2.6氣相層析質譜儀的分析設定條件.........................................................................15
第三章實驗結果與討論...........................................................................................................17
3.1方法的確立.............................................................................................................17
3.1.1定性/定量離子的選用...................................................................................17
3.1.2檢量線的建立................................................................................................25
3.1.3分析方法的確效評估....................................................................................26
3.1.3.1日內及日間變動精密度及準確度.....................................................26
3.1.3.2最低可偵測極限及最低可定量極限(LOD&LOQ) ..........................26
3.1.3.3萃取回收率.........................................................................................26
3.1.3.4基質效應.............................................................................................27
3.1.3.5線性關係.............................................................................................28
3.1.3.6應用於市售茶飲之檢測.....................................................................28
第四章 結論.............................................................................................................................34
參考文獻...................................................................................................................................35
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