- 學位論文
農產品中Neonicotinoids殺蟲劑多重殘留分析方法之探討
Studies on the Multiresidue Determination of Neonicotinoids in Crops
摘要
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。
關鍵字
Neonicotinoids並列摘要
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 .