Flupyradifurone is a new class of butenolide insecticide. As an alternative to imidacloprid, flupyradifurone will be widely used to remove sucking insect pests. This study was conducted to develop a new method for the residues of flupyradifurone in mandarin and pepper. They were suggested as the food commodities to determine the maximum residue limits (MRLs) in Korea. The analyte was analyzed and quantified by gas chromatography equipped with electron capture detector (GC-ECD). Samples were extracted by acetonitrile and purified through silica solid phase extraction (SPE) cartridge. The linearity was good with a determination coefficient ( r2>0.99). Limit of detection(LOD) and limit of quantification(LOQ) were 0.001 and 0.005mg/kg, respectively. Recovery tests were conducted at three concentration levels (LOQ, 10×LOQ, 50×LOQ, n=5). The recovery rates of flupyradifurone were from 71.2 to 114.6% with relative standard deviations(RSDs) less than 9%. All values were consistent with the ranges required in the CODEX guidelines(CAC/GL40). The proposed method was effective and suitable to determine the residues of flupyradifurone in mandarin and pepper.
이 연구는 축산물 중 포레이트 및 대사산물 5종의 안전관리를 위한 공정분석법을 확립하기 위하여 수행하였으며 분석법의 선택성, 검출한계 및 정량한계, 회수율에 대한 검증을 통하여 포레이트 및 대사산물 5종의 공정시험법으로의 유효성을 확인하였다. 포레이트 및 대사산물 5종을 신속하고 효과적으로 동시에 분석하기 위하여 LC-MS/MS를 사용하였고, 1% 아세트산 포함 아세토니트릴 추출 후PSA, C18을 이용해 정제하였다. 개발된 분석법의 평균 회수율은 79.2-113.9%였으며, 분석오차는 19.2% 이하로 정확성 및 재현성이 우수함을 확인할 수 있었다. 개발된 분석법은 국제적 잔류농약 분석 가이드라인에 적합한 수준이었으며 축산물 중 포레이트 및 대사산물 5종의 잔류검사를 위한 공정분석법으로 활용할 수 있을 것으로 판단된다.
Uptake of the triazole fungicides, fluquinconazole and tetraconazole from shoot part of onion was assessed by determining residual amounts of applied fungicides in edible and shoot parts of onion after the foliar application. Combined product of fluquinconazole and tetraconazole (14:7, v/v) as a 21% active ingredient of suspended emulsion formulation was diluted at ratio of 500 and 200 times and sprayed on the shoot part of onion after sealing its root part with absorbent paper. At 10 days after the pesticide application, fluquinconazole residue in the shoot part was the greatest as 5.2 mg/kg at 200 times-dilution treatment, while tetraconazole residue in this part was the smallest as 1.2 mg/kg at 500 times-dilution treatment. On the other hand, the pesticide residues in edible parts of onion at all the treatments were less than limits of detection, 0.01 mg/kg. However, fluquinconazole residues in the edible part of onion divided into three groups such as 1st, 2nd, and 3rd layers were detected at concentrations of 0.04 or 0.24 mg/kg, and these results show the different distribution of pesticides in onion depending on divided layers. In addition, chopped onions were soaked in pesticide solutions prepared with dilution of 1,000 times, cooked using three food processing types such as boiling, stir frying, and pickling, and the pesticide residues in them were analyzed. The analyzed results showed the largest pesticide dissipation in onion followed boiling process (76.9~92.6%).
Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatographelectron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination (r 2 ) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.
A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination (r 2 ) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.
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