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研究生:吳克慧
研究生(外文):Ko-Hui Wu
論文名稱:農產品中Neonicotinoids殺蟲劑多重殘留分析方法之探討
論文名稱(外文):Studies on the Multiresidue Determination of Neonicotinoids in Crops
指導教授:吳明忠吳明忠引用關係
指導教授(外文):Ming-Jung Wu
學位類別:碩士
校院名稱:高雄醫學大學
系所名稱:藥學研究所碩士班
學門:醫藥衛生學門
學類:藥學學類
論文種類:學術論文
論文出版年:2004
畢業學年度:93
語文別:中文
論文頁數:68
中文關鍵詞:Neonicotinoids
外文關鍵詞:Neonicotinoids
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本研究建立以高效液相層析法,同時檢測農產品中:亞滅培、可尼丁、益達胺及賽速安等四種neonicotinoids殺蟲劑殘留量之檢驗方法。檢體以乙腈均質萃取,經過濾、減壓濃縮及graphitized carbon過濾層析匣淨化,最後利用高效液相層析儀分析定量。所使用的液相層析管柱為Inertsil 5 ODS-3V (15 cm×4.6 mm i.d., 5 µm),並採用乙腈與水(含40mM磷酸二氫鉀及5mM 1-己烷磺酸鈉)(25:75, v/v)溶液為移動相溶液,於紫外光檢測器254 nm進行偵測。經以0.02 ~ 4.0 µg/mL之四種混合標準溶液所製作標準曲線的相關係數,皆大於0.999。添加neonicotinoids相當於0.05、0.5及1.0 ppm三種濃度於小黃瓜、蕃茄、水梨、木瓜、米及茶葉檢體中之平均回收率介於80.01~102.12%之間。變異係數皆小於5.0%,本方法最低檢出限量於蔬果及米為0.02 ppm、茶葉為0.2 ppm。同日內與異日間之變異係數分別小於1.78%及3.94%,顯示本方法之精密度可接受。進而利用本方法分析市售蔬果、米及茶葉等20件檢體,結果均未檢出neonicotinoids之殘留。
A high performance liquid chromatographic (HPLC) method for determining Acetamiprid, Clothianidin, Imidacloprid and Thiamethoxam residues in crop was developed. Residues of these four neonicotinoids were extracted with acetonitrile under basic conditions, followed by a graphitized carbon cartridge clean-up procedure . The HPLC separation was achieved on a Inertsil 5 ODS-3V(15 cm×4.6 mm i.d.,5 µm), using with acetonitrile and H2O (40 mM potassium dihydrogen phosphate and 5mM sodium 1-hexanesulfonate), and detection at UV 254 nm. Good linearity was observed from the calibration plot at concentrations from 0.02 to 4.0 µg/mL. Recovery studies of the analytes were performed at 0.05, 0.5 and 1.0 ppm spiked levels. Average recoveries of four neonicotinoids ranged from 80.01 to 102.12% with coefficients of variation less than 5.0%. The detection limits of neonicotinoids were 0.02 ppm in the vegetables, fruits, rice and 0.2 ppm in tea leaf with UV detection. The coefficients of variation of intra-day and inter-day assays were lower than 1.78% and 3.94%, respectively. These results indicated that the developed method had an acceptable precision. Using this method to detect neonicotinoids in 20 samples of vegetables, fruits, rice and teas purchased from various markets in Kaohsiung, the results showed that the four neonicotinoids were not detected in all samples .
中文摘要………………………………………………………………..4
英文摘要………………………………………………………………..5
壹、前言………………………………………………………………..6
貳、文獻回顧……………………………………………………….…..8
一、農藥藥效主成份之發展趨勢………………………………….8
二、我國農藥殘留量監測現況…………………………………….9
三、Neonicotinoids之限量標準…………………………………....10
四、Neonicotinoids之多重分析方法之回顧……………………….10
五、對偶離子層析法……………………………………………….12
六、文獻回顧之圖表………………………………………………..15
參、材料與方法…………………………………………………….…..27
一、檢體來源………………………………………………………..27
二、化學藥品………………………………………………………27
三、儀器設備與裝置………………………………………………27
四、40mM磷酸二氫鉀溶液及5mM 1-己烷磺酸鈉之調製……….28
五、標準溶液之調製……………………………………………….28
六、分析方法……………………………………………………….28
七、回收試驗……………………………………………………….30
八、最低檢出限量………………………………………………….30
肆、結果與討論………………………………………………………..31
一、初期討論………………………………………………………31
二、高效液相層析條件之探討…………………………………….31
三、前處理之探討…………………………………………………32
四、標準曲線……………………………………………………….34
五、回收試驗及最低檢出限量…………………………..………...34
六、同日內與異日間之重複性………………………………….34
七、本研究所建立之檢驗方法與前人研究之比較……………..35
八、市售農產品中Neonicotinoids之多重殘留量調查…………35
伍、結論……………………………………………………………….36
陸、參考文獻…………………………………………………………..37
柒、本研究之圖表……………………………….…..………………..51
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