開發毛細管電泳檢測稻米中殘留農藥的分析技術.doc

中文摘要 本研究利用毛細管電泳結合紫外可見光吸收偵測器(簡稱CE-UV)開發一種快速分離及簡易偵測胺基甲酸鹽類農藥(滅必蝨、加保扶及其代謝物三酮基加保扶、三羥基加保扶、丁基加保扶)的方法。本實驗分別針對緩衝溶液、以及做探討，在毛細管方面使用內徑75 μm，外徑375 μm，全長60 cm，有效長度為50 cm之毛細管，最佳分離條件為20 mM 磷酸緩衝溶液(pH 8.0)並添加15 mM SDS作為電泳緩衝溶液，UV偵測器偵測波長設定於200 nm，電壓+12.5 kV下，進行電泳，可在15分鐘內完成分離。以訊號/雜訊比(S/N ration)等於3作為判定標準，估算本方法最低偵測極限(LOD)可達0.235 ppm (三酮基加保扶)，最高為3.81 ppm (丁基加保扶)，且五種分析物的R2值皆在0.995以上，並且比較同一天及不同天偵測出的RSD值皆小於5% 以下。將本方法應用在市面上的農藥(加保扶)偵測上，無需特殊前處理步驟，可在無基質干擾的狀態下，成功的偵測及定量加保扶，將市售樣品以去離子水稀釋105倍所測得的加保扶含量為1.8×10-5 M，回推濃度與樣品標示相符合，RSD值為2.28% (n = 3)，且偵測加保扶含量與物品標示含量誤差值只有0.13%。應用在真實樣品稻米上，前處理方式以現行日本公告的前處理方法，並利用固相萃取法過濾，得以減少基質干擾並加以淨化達到分析的效果，並於上機前添加0.5 ppm 的加保扶，可以成功測得所公告最高殘留容許量標準為0.5 ppm，RSD值為1.4% (n = 3)，且回收率可達到95.54%。驗證此分析方法可應用在市售農藥及稻米成品中農藥的偵測及定量。 、毛細管電泳 英文摘要 In this study, we developed an analytical method for five pesticides (carbofuran, isoprocarb, and some of their mainmetabolites, carbofuran-3-hydroxy, carbofuran-3-keto, carbosulfan) by using micellar electrokinetic chromatography (MEKC). Aspects of capillary electrophoresis use of diameter 75 μm, outer diameter 375 μm length 60 cm, effective length of 50 cm of the capillary. The optimum separation conditions for MEKC were 20 mM phosphate buffer (pH 8.0) containing 15 mM sodium dodecyl sulfate (SDS). UV detectors measured wavelength set 200 nm,under +12.5 kV electrophoresis. Under this condition, these pesticides were separated for less than 15 min and the detection limit indistilled water were 1μM (carbofuran, isoprocarb, 3-hydroxy-carbofuran, 3-keto-carbofuran), 1μM (carbosulfan) respectively.The linear ranges of the five pesticides were 1 μM to 50 μM (carbofuran, isoprocarb, 3-hydroxy-carbofuran, 3-keto-carbofuran), 10 μM to 100 μM (carbosulfan) with R2 all larger than 0.995. This method was applied to not only the analysis of the residual pesticides in rice sample without pretreatment but also the analysis of commercial insecticide (carbofuran). The results revealed that the recovery for rice sample samples and the carbofuran contains in rice sample