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- 저자 : 고아영(Ah-Young Ko) (검색결과 15 건)
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GC-ECD를 이용한 농산물 중 제초제 aclonifen의 공정분석법 확립
고아영 ( Ah Young Ko ),김희정 ( Hee Jung Kim ),장진 ( Jin Jang ),이은향 ( Eun Hyang Lee ),주윤지 ( Yoon Ji Joo ),권찬혁 ( Chan Hyeok Kwon ),손영욱 ( Young Wook Son ),장문익 ( Moon Ik Chang ),이규식 ( Gyu Seek Rhee ) 한국환경농학회 2014 한국환경농학회지 Vol.33 No.4
BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10×LOQ, 50×LOQ, n=5). Therecoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.
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LC-MS/MS를 이용한 농산물 중 Isoxaflutole과 대사산물(Diketonitrile)의 동시시험법 개발
고아영(Ah-Young Ko),김희정(Heejung Kim),도정아(Jung Ah Do),장진(Jin Jang),이은향(Eun-Hyang Lee),주윤지(Yunji Ju),김지영(Ji Young Kim),장문익(Moon-Ik Chang),이규식(Gyu-Seek Rhee) 한국농약과학회 2016 농약과학회지 Vol.20 No.2
A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges (0.02-2.0 ㎍/mL) for all the analytes into blank extract with r2 > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.
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LC-MS/MS를 이용한 농산물 중 Cyclaniliprole과 대사산물의 동시시험법 개발
도정아 ( Jung-ah Do ),고아영 ( Ah-young Ko ),장진 ( Jin Jang ),주윤지 ( Yunji Ju ),임승희 ( Seung-hee Lim ),박신민 ( Shin Min Park ),장문익 ( Moon-ik Chang ),이규식 ( Gyu-seek Rhee ) 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-
Cyclaniliprole은 2004년 일본 Ishihara Sangyo Kaisha(ISK) Ltd.에서 개발한 diamide계 살충제로 나비목, 총채벌레류, 굴파리류에 대해 높은 살충효과를 갖는 약제이다. 작용기작은 경구 및 경피를 통해 해충의 체내에 흡수되어 신속히 먹이 활동을 정지시키고, 근육세포에 존재하는 리아노딘 수용체를 활성화시켜 근소포체의 Ca2+ 이온을 이상 생산하며, 근육의 경련이나 위축을 일으켜 살충 활성을 나타내는 것으로 알려져 있다. Cyclaniliprole은 생물 및 작물에 대한 안전성을 확인하여 유럽, 미국, 아시아 등에 등록신청이 진행 중이며 국내에서도 2016년 고추, 배추, 파에 대해 등록 요청된 신규 농약이다. Cyclaniliprole은 식물 체내에서 2종의 대사산물(NK-1375, YT-1284)을 형성하는데 그 중 NK-1375는 총잔류방사능(TRR)이 10% 이상으로 검출되었고, 작물잔류성시험에서도 잔류성이 확인되어 모화합물과 함께 관리해야 한다. 따라서 본 연구에서는 cyclaniliprole 및 NK-1375의 동시 동시분석을 위한 공정시험법을 개발하고자 하였다. 또한 범용적 잔류농약 검사가 가능하도록 대표농산물 5종(감귤, 고추, 감자, 현미, 대두)을 이용하여 cyclaniliprole 및 NK-1375를 acetonitrile로 추출하였고, 이온화를 억압하여 유기 용매에 대한 분배효율을 높이기 위해 1 N HCl을 이용하여 pH를 3으로 조절한 뒤 dichloromethane으로 액-액 분배하였으며 유지시료는 n-hexane/acetonitrile 분배법을 추가하여 유지성분을 제거한 뒤 분석하였다. 분석기기는 모화합물의 열분해성과 대사산물의 간섭 영향을 고려하여 선택성이 높고 분석 감도가 우수한 LC-MS/MS를 이용하여 잔류물의 정확성 및 신뢰성을 동시에 확보하였다. 시험법의 검량선 상관계수(r2)는 0.99 이상으로 우수한 직선성을 나타냈고, 정량한계(LOQ)는 0.005 mg/kg으로 미량 정량이 가능하였다. 대표농산물에 LOQ, LOQ 10배, LOQ 50배 수준(0.005, 0.05, 0.25 mg/kg, n=5)으로 회수율 실험을 수행한 결과, 평균 회수율은 cyclaniliprole 81.2-111.5%, NK-1375 76.2-109.2%로 확인되었고, 상대표준편차는 9.4% 미만으로 조사되었다. 개발된 시험법은 국제식품규격위원회(CODEX)의 농약 시험법 가이드라인(CAC/GL 40, 2003)에 부합한 것으로 확인되어 국내 유통되는 농산물 중 cyclaniliprole의 잔류물 안전관리를 위한 공정시험법으로 활용할 수 있을 것으로 판단된다.
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LC-MS/MS를 이용한 농산물 중 식물생장조절제 Trinexapac-ethyl과 대사산물 Trinexapac의 동시분석법 개발
장진 ( Jin Jang ),김희정 ( Hee Jung Kim ),고아영 ( Ah Young Ko ),이은향 ( Eun Hyang Lee ),주윤지 ( Yun Ji Ju ),장문익 ( Moon Ik Chang ),이규식 ( Gyu Seek Rhee ),서세정 ( Sae Jung Suh ) 한국환경농학회 2015 한국환경농학회지 Vol.34 No.4
BACKGROUND: Trinexapac-ethyl is a plant growth regulator (PGR) that inhibits the biosynthesis of plant growth hormone (gibberellin). It is used for the prevention of lodging, increasing yields of cereals, and reducing mowing of turf. The experiment was conducted to establish a determination method for trinexapac-ethyl and its metabolites trinexapac in agricultural products using LC-MS/MS.METHODS AND RESULTS: Trinexapac-ethyl and trinexapac were extracted from agricultural products with methanol/distilled water and the extract was partitioned with dichloromethane and then detected by LC-MS/MS. Limit of detection(LOD) was 0.003 mg/kg and limit of quantification(LOQ) was 0.01 mg/kg, respectively. Matrix matched calibration curves were linear over the calibration ranges (0.01-1.0 mg/L) for all the analytes into blank extract with r2 > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, 50LOQ, n=5). Recoveries of trinexapacethyl and trinexapac were within the range of 73.6-106.9%,72.7-99.2%, respectively. The relative standard deviations (RSDs) were less than 9.0%. All values were consistent with the criteria ranges requested in the CODEX guideline(CAC/GL 40, 2003).CONCLUSION: The proposed analytical method was accurate, effective and sensitive for trinexapac-ethyl and trinexapac determination and it can be used to as an official method in Korea.
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농식품 환경 분야(PF) : PF-09 ; GC-ECD를 이용한 감귤과 고추 중 플루피라디퓨론의 분석법 개발
김희정 ( Heejung Kim ),이은향 ( Eun Hyang Lee ),고아영 ( Ah Young Ko ),장진 ( Jin Jang ),이지영 ( Ji Young Lee ),이상목 ( Sang Mok Lee ),조윤제 ( Yun Je Cho ),장문익 ( Moon Ik Chang ),정지윤 ( Ji Yun Jung ),이은주 ( Eun Ju Lee ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
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.
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HPLC-UVD를 이용한 농산물 중 Imazapyr의 공정분석법 확립
장진(Jin Jang),김희정(Heejung Kim),고아영(Ah-Young Ko),이은향(Eun-Hyang Lee),주윤지(Yoon Ji Joo),김진홍(Jinhong Kim),장문익(Moon-Ik Chang),이규식(Gyu-Seek Rhee) 한국농약과학회 2015 농약과학회지 Vol.19 No.1
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<SUP>2</SUP>) 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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