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GC-MS/MS를 이용한 갈색거저리 유충 중 Chlorpyrifos-methyl과 Deltamethrin의 잔류분석법 확립
백수진 ( Sujin Baek ),김이선 ( Leesun Kim ),손경애 ( Kyungae Son ),노현호 ( Hyunho Noh ),문병철 ( Byeong-chul Moon ),김단비 ( Danbi Kim ),오민석 ( Min-seok Oh ),노진호 ( Jin-ho Ro ),김은선 ( Eunsun Kim ) 한국환경농학회 2020 한국환경농학회 학술대회집 Vol.2020 No.-
Nowadays, edible insects are spotlighted as future food in the Korean local market due to its high protein contents. However, food safety for edible insects should be guaranteed. Therefore, this study was aimed to establish the analytical method of chlorpyrifos-methyl and deltamethrin in mealworms to provide data for guidelines on safety of edible insects. The sample preparation was based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) EN method. For extraction efficiency, acetonitrile (ACN) instead of ACN containing 0.1% formic acid were investigated. To compare cleanup methods, MgSO<sub>4</sub>, PSA, C18, EMR-lipid ™ and n-hexane were applied to remove protein and fat. After establishing the final analytical method, the control samples were spiked at two levels (10 ㎍/kg, 100 ㎍/kg) and the recovery tests were performed as follows. Five grams of samples were extracted by 10 mL of ACN and added with MgSO<sub>4</sub> 4g, NaCl 1g, NaCitrate 1g and disodium citrate sesquihydrate 0.5g for partitioning. Finally, dispersive-solid phase extraction (MgSO<sub>4</sub> 150mg, PSA 25mg, and C18 25mg) was selected for rapid and efficient cleanup. The samples were analyzed by gas chromatography tandem mass spectrometry. The method limit of quantification of chlorpyrifos-methyl and deltamethrin were 2.5㎍/L and the correlation coefficient (r2) of calibration curve were > 0.99. The recoveries of chloropyrifos-methyl were 82.5 - 114.0 ± 1.6 -3.0% and deltamethrin were 84.9-93.8 ± 5.7 - 6.5 %. Two target pesticides were not detected in the real samples (n=30) of edible insects collected to monitor in South Korea. These results can be useful data for guidelines on safety of mealworms to prepare Positive List System in South Korea.
LC-MS/MS를 이용한 갈색거저리 유충 중 Fenoxanil, Thiobencarb 및 Fludioxonil의 잔류분석
김이선 ( Leesun Kim ),백수진 ( Sujin Baek ),손경애 ( Kyungae Son ),노현호 ( Hyunho Noh ),문병철 ( Byeong-chul Moon ),김단비 ( Danbi Kim ),오민석 ( Min-seok Oh ),노진호 ( Jin-ho Ro ),김은선 ( Eunsun Kim ) 한국환경농학회 2020 한국환경농학회 학술대회집 Vol.2020 No.-
This study was designed to determine fenoxanil, thiobencarb, and fludioxonil residues in mealworms, the larvae of Tenebrio moliter using liquid chromatography tandem mass spectrometry. These pesticides are officially applied for wheat cultivation, so can be found in wheat bran, recommended feed for mealworms in South Korea. In this regard, effective analytical method is urgently required because mealworms are used as food or feed as alternative protein sources. Acetonitrile (10 mL) was used to extract the target pesticides. Four clean-up procedures ((1) MgSO<sub>4</sub>+25 mg PSA+25 mg C18 (2) MgSO<sub>4</sub>+50 mg PSA+50 mg C18 (3) EMR-lipid™ tube, and (4) 10 mL n-hexane) were examined. The procedure (1) successfully removed lipids and proteins derived from insects with the satisfied recoveries of the target analytes at two spiking levels of 5 ㎍/kg and 10 ㎍/kg. The recoveries were 87.6-112.9 ± RSD 4.2-4.6% for fenoxanil, 83.3-87.6 ± RSD 1.3-4.6% for thiobencarb, and 76.9~82.0 ± RSD 3.4-7.2% for fludioxonil. Method detection limit was 1.0 Mg/L. The optimized method was also applied to real samples from 30 different farms across the nation. These data can be used to set maximum residual limit for the residues in edible insects in response to positive list system. The method developed in this study is expected to be also applied to other edible insects or matrices having high fat and protein contents.