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엇갈이배추 재배기간 중 살균제 Amisulbrom의 생산단계 잔류허용기준 설정
안경근 ( Kyung Geun Ahn ),김경하 ( Gyeong Ha Kim ),김기쁨 ( Gi Ppeum Kim ),김민지 ( Min Ji Kim ),홍승범 ( Seung Beom Hong ),황영선 ( Young Sun Hwang ),권찬혁 ( Chan Hyeok Kwon ),손영욱 ( Young Wook Son ),이영득 ( Young Deuk Lee 한국환경농학회 2015 한국환경농학회지 Vol.34 No.2
BACKGROUND: Supervised residue trials were conducted to establish pre-harvest residue limit(PHRL), a criterion to ensure the safety of the pesticide residue in the crop harvest, of amisulbrom for winter-grown cabbage in two fields. Following to application of amisulbrom on the crop, time-course study was carried out to obtain the amisulbrom dissipation of statistical significance which enabled to calculate the predicted values of PHRL. METHOD AND RESULTS: During cultivation under greenhouse condition, samples of winter-grown cabbage were collected at 0, 1, 3, 5, 7 and 10 days after amisulbrom application, and subjected to residue analysis. Analytical method was validated by recoveries ranging 93.7~100.0% as well as limit of quantitation(LOQ) of 0.04 mg/kg. Amisulbrom residues in winter-grown cabbage gradually decreased as time elapsed. The dissipation rate of the residue would be affected by intrinsic degradation along with dilution by the cabbage growth. The decay pattern was well fitted by the simple first-order kinetics. CONCLUSION: Biological half-lives of amisulbrom in winter-grown cabbage ranged 3.7~4.1 days in two field conditions. Based on the regression of amisulbrom dissipation, PHRLs of amisulbrom in winter-grown cabbage were recommended as 8.86~9.47 and 4.21~4.35mg/kg for 10 and 5 days before harvest, respectively.
안경근 ( Kyung Geun Ahn ),김기쁨 ( Gi Ppeum Kim ),황영선 ( Young Sun Hwang ),강인규 ( In Kyu Kang ),이영득 ( Young Deuk Lee ),정명근 ( Myoung Gun Choung ) 한국환경농학회 2018 한국환경농학회지 Vol.37 No.2
BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.
GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석
안경근(Kyung-Geun Ahn),김경하(Gyeong-Ha Kim),김기쁨(Gi-Ppeum Kim),황영선(Young-Sun Hwang),홍승범(Seung-Beom Hong),이영득(Young Deuk Lee),정명근(Myoung-Gun Choung) 한국농약과학회 2015 농약과학회지 Vol.19 No.3
Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930’s as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.
06 식품의약품안전처 SESSION : GC-NPD/MS를 이용한 농산물 중 유기인계 농약의 동시분석법 확립
안경근 ( Kyung Geun Ahn ),김경하 ( Gyeong Ha Kim ),김기쁨 ( Gi Ppeum Kim ),김민지 ( Min Ji Kim ),김슬아 ( Seula Kim ),강련웅 ( Ryeon Woong Kang ),김정은 ( Jeong Un Kim ),황영선 ( Young Sun Hwang ),이영득 ( Young Deuk Lee ),정명근 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
본 연구는 유기인계 농약 중 제초제 anilofos, 살균제 iprobenfos, 살충제인 chlorpyrifos-methyl,mecarbam, parathion-methyl, phenthoate, prothiofos 및 tebupirimfos 등 8종 농약의 동시분석법을 개발하고자 하였다. 현재 식품공전에 수록되어 있는 이들 각 농약의 기기분석법은 GC-ECD,GC-NPD 혹은 GC-FPD 분석법이 각각 적용되어 있으므로 고감도 선택성 검출기의 적용이 필요하며, 아울러 기존 분석법은 packed column의 사용 및 cartridge 정제에 의해 정제도 및 재현성 불량 등 일상분석에 어려움이 있으므로, 본 연구는 농축, 유지제거 과정 및 정제과정의 간소화를 통해 보다 편리하고, 신뢰성 높은 GC-NPD/MS 분석법을 확립하고자 하였다. 부류별 5종(현미, 콩, 배추, 감귤 및 고추)의 대표 농산물을 선정하여 마쇄 후 아세톤으로 추출하고, 포화식염수와 증류수를 첨가한 뒤 n-hexane으로 액-액 분배하여 florisil 흡착크로마토그래피법으로 정제하였다. Florisil 정제법은 50 mL의 n-hexane/acetone(99.5:0.5, v/v)으로 세척한 후 150 mL의 n-hexane/ acetone (97:3, v/v)로 용출하여 chlorpyrifos-methyl, mecarbam, parathion-methyl, phenthoate, prothiofos 및 tebupirimfos의 6성분을 분리하였고, 추가적으로 150 mL의 n-hexane/acetone(92:8, v/v)로 anilofos 및 iprobenfos 2성분을 용출하였다. 분석대상 농약의 기기분석 시 resolution을 고려하여 최적의 분석용 GC 컬럼은 DB-17 capillary column으로 선정하였으며, 3수준 3반복으로 실험을 수행한 결과, 정량한계는 chlorpyrifos-methyl, parathion-methyl 및 tebupirimfos이 0.004 mg/kg, 그외 anilofos, iprobenfos, mecarbam, phenthoate 및 prothiofos는 0.008 mg/kg이었다. 각 대표 농산물에 대해 정량한계, 정량한계 10배 및 50배 수준에서 회수율을 검정한 결과, 모든 처리농도에서 80.7-105.0%의 회수율을 나타내었으며, 반복 간 변이계수(CV)는 최대 5.8% 미만으로 잔류분석 기준인 회수율 70-120% 및 분석오차 10% 이내를 만족하였다. 또한 GC/MS를 통해 잔류분을 재확인 하였으며, TIC(Total-Ion Chromatogram)와 mass spectrum을 고려하여 SIM (Selected-Ion Monitoring)을 통해 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로서 GC-NPD/MS를 이용한 유기인계 농약 anilofos, iprobenfos, chlorpyrifos-methyl, mecarbam, parathion-methyl, phenthoate, prothiofos 및 tebupirimfos의 동시분석법은 재현성 및 신뢰성이 확보된 정밀 분석법으로써, 일상적잔류 농약분석에 적용 가능할 것으로 판단된다.
HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석
안경근(Kyung-Geun Ahn),김경하(Gyeong-Ha Kim),김기쁨(Gi-Ppeum Kim),김민지(Min-Ji Kim),황영선(Young-Sun Hwang),홍승범(Seung-Beom Hong),이영득(Young Deuk Lee),정명근(Myoung-Gun Choung) 한국농약과학회 2014 농약과학회지 Vol.18 No.4
This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.
식품의약품안전처 SESSION : GC/ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석
안경근 ( Kyung Geun Ahn ),김기쁨 ( Gi Ppeum Kim ),조영욱 ( Young Wook Cho ),황영선 ( Young Sun Hwang ),이수진 ( Su Jin Lee ),윤원갑 ( Won Kap Yun ),강민주 ( Min Ju Kang ),김슬아 ( Seula Kim ),이영득 ( Young Deuk Lee ),정명근 ( Myo 한국환경농학회 2013 한국환경농학회 학술대회집 Vol.2013 No.-
Quintozene, pentachloronitrobenzene(PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930`s as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea in 1969 but now banned to use due to its high residue levels in selected harvests, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Chinese cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.
주요 농산물 중 Bezenesulfonamide계 살균제 Flusulfamide의 잔류 분석법
안경근 ( Kyung-geun Ahn ),김기쁨 ( Gi-ppeum Kim ),황영선 ( Young-sun Hwang ),강인규 ( In-kyu Kang ),이영득 ( Young Deuk Lee ),정명근 ( Myoung-gun Choung ) 한국환경농학회 2018 한국환경농학회지 Vol.37 No.1
BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.
GC-ECD/MS를 이용한 농산물 중 Fipronil의 잔류 분석법 개발
안경근 ( Kyung Geun Ahn ),김경하 ( Gyeong Ha Kim ),김기쁨 ( Gi Ppeum Kim ),황영선 ( Young Sun Hwang ),강인규 ( In Kyu Kang ),이영득 ( Young Deuk Lee ),정명근 ( Myoung Gun Choung ) 한국환경농학회 2015 한국환경농학회지 Vol.34 No.4
BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column.Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities.The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.
수출입 원예작물의 검역을 위한 살균제 Fluazinam의 공정 잔류분석법 개발
김경하(Gyeong-Ha Kim),안경근(Kyung-Geun Ahn),김기쁨(Gi-Ppeum Kim),황영선(Young-Sun Hwang),장문익(Moon-Ik Chang),강인규(In-Kyu Kang),이영득(Young Deuk Lee),정명근(Myoung-Gun Choung) 한국원예학회 2016 원예과학기술지 Vol.34 No.1
This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was 0.004 mgㆍkg<SUP>-1</SUP> in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.
가열조리 시 버섯류 함유 수용성 비타민 B6의 함량 변화
김기쁨 ( Gi-ppeum Kim ),안경근 ( Kyung-geun Ahn ),강련웅 ( Ryeon-woong Kang ),권희주 ( Heeju Kwon ),김명현 ( Myunghyun Kim ),황혜지 ( Hyeji Hwang ),주하은 ( Haeun Joo ),황영선 ( Young-sun Hwang ),최용민 ( Youngmin Choi ),김행란 ( 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-
버섯은 특유한 향과 쫄깃한 맛 때문에 세계적으로 널리 사랑받고 있는 식품이다. 특히 버섯은 채식식단에서 결핍되기 쉬운 비타민 B 복합체를 제공할 수 있기 때문에, 채식 위주의 식단에서 결코 빼놓을 수 없는 식품이다. 그러나 수용성 비타민 B6의 경우 버섯에 함유된 함량 정보가 부족한 실정이다. 따라서 본 연구는 농촌진흥청 국립농업과학원 주관 국가 표준 식품성분표(제9개정판) 제작을 위한 식품자원의 비타민 성분구명 및 DB 구축사업의 일환으로 국내 다소비 버섯류 중 일부를 대상으로 수용성 비타민 B6의 함량변화를 HPLC-FLD 분석법으로 평가하였다. 본 연구에 적용한 HPLC-FLD 분석법의 재현성(inter 및 intra-day), 기기분석 시 검출성분의 이론단수, 검량선의 직선성 및 해상도 등 분석 파라미터를 검토한 결과 우수한 재현성 및 분리능을 확인하였다. 버섯류 중표고버섯을 부위별로 조사한 결과, 기둥(0.023±0.000 mg/100 g)부위가 갓(0.017±0.001 mg/100 g)부위보다 높은 함량을 나타내는 것으로 조사되었다. 아울러 표고버섯 기둥 부위를 데쳤을 시, 0.015 0.001 mg/100 g으로 함량이 감소하였고, 갓 부위를 데쳤을 시에는 0.018±0.000 mg/100 g 으로 생것과 차이가 없는 것으로 확인되었다. 기둥 및 갓 부분 모두 말렸을 시, 생것보다 높은 함량을 나타내는 것으로 조사되었다. 한편, 새송이버섯은 0.007±0.000 mg/100 g의 함량을 나타내었으며, 팽이 및 양송이버섯에서는 비타민 B6가 전혀 검출되지 않았다. 이상의 연구결과는 향후 국가 표준 성분식품표의 제작 및 국민 식생활 증진에 기여할 수 있을 것으로 사료된다.