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LC-MS/MS를 이용한 축산물중 kresoxim-methyl 과 BF 490-9 의 동시 분석법 개발
무스픽 ( Md. Musfiqur Rahman ),조일규 ( Il Kyu Cho ),심재한 ( Jae-han Shim ) 한국환경농학회 2018 한국환경농학회 학술대회집 Vol.2018 No.-
An analytical method was developed for simultaneous determination of kresoxim-methyl and its metabolite, BF 490-9 in animal products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted using acetonitrile and salts, and purified using solid phase extraction procedure (dSPE). Limits of detection (LOD) and limits of quantification (LOQ) for kresoxim-methyl and its metabolites in various animal products matrices were 0.0015~0.003 mg/kg and 0.005~0.01 mg/kg respectively. A seven point matrix matched external calibration curve was constructed for both of the analytes. Good linearity was observed with the determination of co-efficient (R2)≥0.999. Method was validated after fortification of target standard to the blank matrix at three different concentration levels (LOQ, 2LOQ, and 10LOQ) with five replicate for each concentration. Average recovery was achieved within the acceptable range (70~120%) with relative standard deviation (RSD)<20%. The method could be used for routine analysis of kresoxim-methyl and its metabolites in animal products.
04 포스터 발표 : 환경 화학 분야(PC) ; PC-14 : LC-MS/MS를 이용한 돼지, 닭고기, 계란중 Phorate와 대사체의 분석법 개발
무스픽 ( Md. Musfiqur Rahman ),김성우 ( Sung Woo Kim ),최정희 ( Jeong Heui Choi ),이영준 ( Young Jun Lee ),압두 ( A. M. Abd El-aty ),팔하 ( Waziha Farha ),정다이 ( Da I Jung ),카빌 ( Md. Humayun Kabir ),임소정 ( So Jeong Im 한국환경농학회 2015 한국환경농학회 학술대회집 Vol.2015 No.-
An analytical method was validated for phorate and its five metabolites (phoratesulfone, phoratesulfoxide, phorateoxon, phorateoxonsulfone, and phorateoxonsulfoxide) in pork, chicken, and egg using LC-MS/MS. The method was validated following MFDS (ministry of food and drug safety, Republic of Korea) official method developed for beef and milk. Extraction was carried out following QuEChERS using acidified acetonitrile and salt and purification was conducted via dSPE using primary secondary amine (PSA) and C18 sorbent. Calibration curve in matrix was linear with determination coefficient (r2) ≥ 0.995 for all of the analyte in three target matrices. Limit of detection (LOD) and quantification (LOQ) were 0.001 and 0.004 mg/kg for all of the matrices. Recovery was performed at three fortification level resulted acceptable values ranging from 74.22 and 119.89% with relative standard deviation (RSD)<6%. The developed method can be applied for routine analysis of phorate and its metabolites in different animal origin.
04 포스터 발표 : 환경 화학 분야(PC) ; PC-16 : GC-μECD를 이용한 상추중 Metrafenone 잔류양상 연구
카빌 ( Md. Humayun Kabir ),임소정 ( So Jeong Im ),무스픽 ( Md. Musfiqur Rahman ),김성우 ( Sung Woo Kim ),최정희 ( Jeong Heui Choi ),압두 ( A. M. Abd El-aty ),팔하 ( Waziha Farha ),정다이 ( Da I Jung ),이영준 ( Young Jun Lee 한국환경농학회 2015 한국환경농학회 학술대회집 Vol.2015 No.-
The dissipation pattern of metrafenone in green leafy vegetables (lettuce) grown under green house condition were investigated using GC-μECD. Residues were extracted using acetone and samples were taken out by liquid-liquid extraction. Matrix component was cleaned by SPE silica cartridge. Calibration curves were linear over the concentration ranges (0.02-5.0 mg/kg) with a determination co-efficient (r2)≥0.999. The limit of detection (LOD) and quantification (LOQ) were 0.006 and 0.02 mg/kg respectively. Recoveries at two fortification level were ranged between 78.5% and 113.3% with relative standard deviation (RSD)<9%. Residues half-life from dissipation pattern of site 1 and 2 double/triple spray was 2.3/2.2 and 4.9/5.0 days respectively. The method was effective and sensitive enough to determine the residue of metrafenone in field-incurred lettuce sample.
04 포스터 발표 : 환경 화학 분야(PC) ; PC-15 : GC-μECD를 이용한 상추중 Metrafenone과 Boscalid분석을 위한 QuEChERS방법 비교
임소정 ( So Jeong Im ),무스픽 ( Md. Musfiqur Rahman ),김성우 ( Sung Woo Kim ),압두 ( A. M. Abd El-aty ),최정희 ( Jeong Heui Choi ),카빌 ( Md. Humayun Kabir ),팔하 ( Waziha Farha ),정다이 ( Da I Jung ),이영준 ( Young Jun Lee 한국환경농학회 2015 한국환경농학회 학술대회집 Vol.2015 No.-
Three versions of the QuEChERS method (quick,easy, cheap, effective, rugged and safe) . the original (unbuffered), modified acetate-buffered, and citrate-buffered versions were compared for thedetermination of metrafenone and boscalid residues in lettuce via gas chromatography-micro electron capture detector (GC-μECD). Onlymodified acetate-buffered version provided acceptable and more consistent recoveries for both of the target analytes than the other versions. Matrix matched calibration curves prepared for the analytes provided good linearity over the calibration ranges with the co-efficient of determination (r2) ≥ 0.998. Limit of detection (LOD) and quantification (LOQ) were 0.003 and 0.01 mg/kg for both of the analytes. Method was validated in triplicate at two fortification level and recovery of modified acetate buffered version was ranges between 77.0 and 88.1% with relative standard deviation (RSD) < 5 for the quantified analytes. The developed method was applied to the field incurred lettuce sample where half-life of metrafenone and boscalid were found 2.6 and 2.9 days respectively for double doses and 3.4 and 3.6 days respectively for triple doses.
축산물 중 4차 암모늄계 제초제 및 생장조정제 (Chlormequat, Diquat dibromide, Paraquat) 분석법 개발
조일규 ( Il Kyu Cho ),설재웅 ( Jae Ung Seo ),무스픽 ( Md. Musfiqur Rahman ),오영곤 ( Young Gon Oh ) 한국환경농학회 2020 한국환경농학회 학술대회집 Vol.2020 No.-
4차 암모늄계 제초제 및 생장조절제 3종 (Chlormequat,Diquat dibromide, Paraquat) 대상으로 새로운 동시 시료조제법을 확립하여 분석효율을 향상시킴과 동시에 개별 또는 동시의 재현성 높은 기기분석조건을 확립하여 분석 신뢰성을 확보하고자 하였다. 대상농약들은 chloride나 bromide 염의 형태로 살포되나 이는 전자적 균형을 맞추기 위한 counter 음이온들이며 실제 유효성분은 양이온 형태이다. 대상 소고기, 돼지고기, 닭고기, 우유, 계란, 지방(포유동물)의 농약 잔류허용기준은 0.01 ~0.5 mg/kg 범위이므로 성분에 따라 정량한계 0.01 mg/kg 이하를 만족하는 고감도 분석법이 요구되었다. 분석기기는 UPLC-ESI-MS/MS (ABsciex Qtrap 4500를 사용하여 positive mode로 분석하였다. LC-MS/MS 기기조건은 Restek Quat (50 mm x 2.1 mm, 3 um) 컬럼을 사용하여 ion-pairing reagent인 10 mM Heptafluorobutyric acid를 사용한 이동상 (Water : Acetonitrile = 95% : 5%) 조건으로 분석하였다. 전 처리는 축산물 시료를 25% Trichloroacetic acid 로 추출하고 원심 분리하여 상층액을 취하는 과정을 2회 반복한 후 암모니아수로 PH를 9-10이 되도록 조절하고 최종 물 50 mL로 정용하여 분석 하였다. 상기 조건에서 Retention time은 Chlormequat은 1.95분이였고 Diquat dibromide sms 4.66분이였으며 Paraquat은 5.58분으로 3성분 모두 분리 되었다. 분석법 정량한계 (Limit of Quantitation, LOQ)는 0.01 mg/kg 이었으며 돼지고기, 닭고기, 우유, 계란에서 Chlormequat, Diquat dibromide, Paraquat의 회수율은 70% 이상 이였다.