Study for Residue Analysis of Fluxametamid in Agricultural Commodities

Kim, Ji Young,Choi, Yoon Ju,Kim, Jong Soo,Kim, Do Hoon,Do, Jung Ah,Jung, Yong Hyun,Lee, Kang Bong,Kim, Hyochin The Korean Society of Environmental Agriculture 2019 한국환경농학회지 Vol.38 No.1

BACKGROUND: Accurate and simple analytical method determining Fluxametamid residue was necessary in various food matrices. Additionally, fulfilment of the international guideline of Codex (Codex Alimentarius Commission CAC/GL 40) was required for the analytical method. In this study, we developed Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) method to determine the Fluxametamid residue in foods. METHODS AND RESULTS: Fluxametamid was extracted with acetonitrile, partitioned and concentrated with dichloromethane. To remove the interferences, silica SPE cartridge was used before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with $C_{18}$ column. Five agricultural commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used as a group representative to verify the method. The liner matrix-matched calibration curves were confirmed with coefficient of determination ($r^2$) greater than 0.99 at calibration range of 0.001-0.25 mg/kg. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. Mean average accuracies were shown to be 82.24-115.27%. The precision was also shown to be less than 10% for all five samples. CONCLUSION: The method investigated in this study was suitable to the Codex guideline for the residue analysis. Thus, this method can be useful for determining the residue in various food matrices as routine analysis.

Study for Residue Analysis of Fluxametamid in Agricultural Commodities

( Ji Young Kim ),( Yoon Ju Choi ),( Jong Soo Kim ),( Do Hoon Kim ),( Jung Ah Do ),( Yong Hyun Jung ),( Kang Bong Lee ),( Hyochin Kim ) 한국환경농학회 2019 한국환경농학회지 Vol.38 No.1

BACKGROUND: Accurate and simple analytical method determining Fluxametamid residue was necessary in various food matrices. Additionally, fulfilment of the international guideline of Codex (Codex Alimentarius Commission CAC/GL 40) was required for the analytical method. In this study, we developed Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) method to determine the Fluxametamid residue in foods. METHODS AND RESULTS: Fluxametamid was extracted with acetonitrile, partitioned and concentrated with dichloromethane. To remove the interferences, silica SPE cartridge was used before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with C18 column. Five agricultural commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used as a group representative to verify the method. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) greater than 0.99 at calibration range of 0.001-0.25 mg/kg. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. Mean average accuracies were shown to be 82.24-115.27%. The precision was also shown to be less than 10% for all five samples. CONCLUSION: The method investigated in this study was suitable to the Codex guideline for the residue analysis. Thus, this method can be useful for determining the residue in various food matrices as routine analysis.

농산물 중 잔류 플루피리민과 그 대사체 분석법 개발

김대원 ( Dae Won Kim ),김지영 ( Ji Young Kim ),김효진 ( Hyochin Kim ),송지영 ( Ji Young Song ),한아름 ( A Reum Han ),김종수 ( Jong Soo Kim ),윤상순 ( Sang Soon Yun ),정용현 ( Yong Hyun Jung ),윤혜정 ( Hae Jung Yoon ),윤은경 ( Eun 한국환경농학회 2020 한국환경농학회 학술대회집 Vol.2020 No.-

Flupyrimin is used for rice plants. Not only it exhibits outstanding pesticidal property, but also it ensures excellent safety for organisms with pollinator by interacting with insectile neurons(nAChR, nicotinic Acetylcholine receptor). In this study, an analytical method for the determination of Flupyrimin and its metabolites residues in foods was developed as Ministry of Food and Drug Safely (MFDS) method. We used five agricultural products (mandarine, potato, soybean, hulled rice, and chilli pepper) as group representative to verify. The sample preparation process was conducted in two steps with QuEChERs method. First, in order to extract the samples, 2% formic acid in acetonitrile was added and shaken for 10 minutes. After that magnesium sulfate and sodium chloride were added, followed by centrifugation (4,700 G) for 10 minutes. Thereafter, to remove the interferences in samples, dispersive-SPE using C18 and magnesium sulfate was performed for 10 minutes before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with C18 column. The linear standard calibration curve were confirmed (coefficient of determination with calibration range). Mean average accuracies of Flupyrimin and its metabolites (Flupyrimin-M1) were shown 85.18~110.66% and 72.36~100.06%, respectively. The precision were also shown less than 10.58% for all five samples. These results are suitable for CODEX guideline for residue analysis (CAC/GL 40). In short, the proposed method for determination of Flupyrimin residue in foods could be utilized as governmental method.

Study for Residue Analysis of Pinoxaden in Agricultural Commodities

Kim, Ji Young,Yoon, Eun Kyung,Kim, Jong Soo,Seong, Nu Ri,Yun, Sang Soon,Jung, Yong Hyun,Oh, Jae Ho,Kim, Hyochin The Korean Society of Environmental Agriculture 2019 한국환경농학회지 Vol.38 No.4

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C₁₈. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

Study for Residue Analysis of Pinoxaden in Agricultural Commodities

( Ji Young Kim ),( Eun Kyung Yoon ),( Jong Soo Kim ),( Nu Ri Seong ),( Sang Soon Yun ),( Yong Hyun Jung ),( Jae Ho Oh ),( Hyochin Kim ) 한국환경농학회 2019 한국환경농학회지 Vol.38 No.4

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation- MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C18. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

농산물 중 Fluxametamid 분석법 개발

김지영 ( Ji Young Kim ),김효진 ( Hyochin Kim ),최윤주 ( Youn Ju Choi ),송지영 ( Ji Young Song ),강혜라 ( Hera Kang ),도정아 ( Jung Ah Do ),정형욱 ( Hyung-wook Chung ),이규식 ( Gyu Seek Rhee ),이순호 ( Soon Ho Lee ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-

Fluxametamid (IUPAC name: 4-[5-(3, 5-dichlorophenyl)-5-(trifluoromethyl)- 4, 5-dihydro-1, 2-oxazol-3-yl]-N-[(methoxyimino)methyl]-2-methylbenzamide) is isoxazoline insecticide and acarcide. An analytical method for the determination of fluxametamid residue in foods was developed as Ministry of Food and Drug Safety (MFDS) method. After extracting with acetonitrile, samples were partitioned and concentrated with dichloromethane. To remove the interferences, silica SPE cartridge was performed before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with C18 column. Five agricultural commodities (mandarin, potato, soybean, brown rice, and hot pepper) were used as group representative to verify. The linear matrix-matched calibration curve were confirmed (coefficient of determination > 0.99 with calibration range 0.01-2.5 mg/kg). Fluxametamid from sample with recoveris range from 82.24~115.27%. The precision were also shown less than 9.54% for all five samples. These spiked recoveries fall well within the recommened mean values in CODEX guideline for residue analysis (CAC/GL 40). Thus this method successfully processes food samples for Fluxametamid utilizing LC-MS/MS method.

LC-MS/MS를 이용한 농산물 중 이미다졸리논계 농약의 시험법 개발

김지영 ( Ji Young Kim ),김효진 ( Hyochin Kim ),송지영 ( Ji Young Song ),한아름 ( A Reum Han ),성누리 ( Nu Ri Sung ),윤상순 ( Sang Soon Yoon ),정용현 ( Yong Hyun Jung ),오재호 ( Jae Ho Oh ),김종수 ( Jong Soo Kim ) 한국환경농학회 2019 한국환경농학회 학술대회집 Vol.2019 No.-

Imidazolinone herbicides (Imazapyr, Imazalil, Imazamox, Imazaquin, Imazapic, Imazamethabenzmethyl and Imazethapyr) control weeds by inhibiting the enzyme acetohydroxyacid synthase(AHAS), also known as acetolactate synthase (ALS). AHAS is critical enzyme for the biosynthesis of branched chain amino acids in plants. Currently, each individual analytical method for Imidazoline herbicides is used as Ministry Food and Drug Safety (MFDS) method. Thus it consumes lots of time and effort to determine residue of Imidazolinone group in food. A Single analytical method for the determination of Imidazolinone residue in foods was developed as Ministry of Food and Drug Safety (MFDS) method. Five agricultural commodities (mandarin, potato, soybean, brown rice, and chilli pepper) were used as group representative to verify. After extracting with 1% formic acid in acetonitrile, samples were partitioned by citrate buffer. To remove the interferences, dispersive-SPE using C18 and PSA was performed before LC-MS/MS (Liquid Chromatography -Tandem Mass Spectrometry). The liner standard calibration curve were confirmed (coefficient of determination with calibration range). Mean average accuracies were shown 72.0~116.6 %. The precision were also shown less than 11.6% for all five samples. Thus, this method is acceptable to CODEX guideline for residue analysis (CAC/GL 40). Is sum, the proposed method for Imidazolinone group residue determination can be suitable for CODEX guidelines and useful as government method.

식품 중 잔류농약 안전관리를 위한 농약 허용물질목록 관리제도 도입

손성완 ( Seong Wan Son ),김진숙 ( Jin-sook Kim ),권찬혁 ( Chan-hyeok Kwon ),김효진 ( Hyochin Kim ) 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-

With a growing global population expected to reach over 9 billion in 2050 and the increasing impact of climate change, developing sustainable agriculture and aquaculture while at the same time ensuring food safety presents great challenges. Not only does it require a better understanding of how terrestrial and aquatic ecosystems function and their interrelationship with the availability of quality water, it requires a shift in the way we managethe ecosystems and the water within them to ensure food security. We have to safeguard and use our ecosystems wisely as they provide the basis of all the environmental services needed to achieve food security which are particularly important for the poor, women, and marginal groups. Agricultural and aquaculture production systems have to be recognized and managed as a landscape of integrated agro ecosystems with the potential for multiple functions. This presentation will review and examine the complexities involved in our ability to grow food sustainably in the midst of the degradation of the ecosystem services and examine the role policy makers can play in encouraging producers to retain or adopt more susceptible farming practices while safeguarding the benefits for local, national and global populations.

농산물 중 잔류 아이소사이클로세람과 그 대사체 식품공전 분석법 개발

이유선 ( Yu Seon Lee ),김지영 ( Ji Young Kim ),김효진 ( Hyochin Kim ),이정은 ( Jeong Eun Lee ),송영빈 ( Young Bin Song ),이정미 ( Jung Mi Lee ),정용현 ( Yong-hyun Jung ),문귀임 ( Gui Im Moon ),허수정 ( Soo Jung Hu ),강길진 ( Gil J 한국환경농학회 2021 한국환경농학회 학술대회집 Vol.2021 No.-

As a insecticide belonged isoxazoline class, Isocycloseram is an active chemical against lepidoptera, true bugs and beetles. Also, this chemical acts as a noncompetitive inhibitor for γ-aminobutyric acid(GABA) receptor of invertebrates. In this study, an Korea governmental official analytical method, Ministry of Food and Drug Safety (MFDS) method, for the determination of Isocycloseram and its metabolites residues (SYN549431, SYN548569) in foods and agricultural products was developed. Five agricultural products (mandarine, potato, soybean, hulled rice, and chilli pepper) as group representative to verify was used in this study. The sample preparation process was conducted in two steps with "quick, easy, cheap, effective, rugged, and safe (QuEChERs) method". First, in order to extract the samples, 0.1% formic acid in acetonitrile was added and shaken for 10 minutes. Next, magnesium sulfate anhydrous and sodium chloride were added, followed by centrifugation (4,700 G, 10 minutes). Thereafter, to remove the interferences in samples, dispersive-SPE using C18 and magnesium sulfate anhydrous was performed for 10 minutes before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with C18 column. The linear standard calibration curve were confirmed (coefficient of determination with calibration range). Mean average accuracies of Isocycloseram and its metabolites were shown 72.0∼109.8%, 71.5∼ 109.6% and 81.9∼106.9% respectively. The precision were also shown less than 10.80% for all five samples. These results are suitable for CODEX guideline for residue analysis (CAC/GL 40). In sum, the proposed method for determination of Isocycloseram and its metabolites residues residue in foods could be utilized as a governmental official method.