• 한국식품과학회지
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• 제37권4호
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• pp.685-694
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• 2005

Korean practices in tolerance setting of pesticide residues on food crops were compiled with an effort to harmonize with international standards. Based on scientific data including historical background, limit setting protocols, adoption of ADI values, food factors, nation's body weights, and regulatory margins which are required for the setting of maximum residue limits, necessary measures to be taken by Korean regulatory authorities were proposed.

• 한국환경농학회지
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• 제24권1호
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• pp.45-55
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• 2005

This study was undertaken to find out necessary measures to improve the tolerance setting system of pesticide residues on food crops in Korea which is scientifically reasonable and harmonizable with international standards. Information on tolerance setting systems of pesticide residues by Codex Alimentarius Commission, Joint FAO/WHO Meeting of Experts on Pesticide Residues, USA, EU, Japan and Taiwan was collected and analyzed. On the basis of information in the above countries, necessary actions to be taken by the Korean regulatory authorities were recommended with respect to priority setting, maximum residue limits (MRLs) setting based on field residue data, group MRLs, minor crop problems, quantitation limit and dietary intake assessment.

• 한국환경농학회지
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• 제38권1호
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• pp.1-9
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• 2019

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.

• 한국환경농학회지
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• 제38권4호
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• pp.321-331
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• 2019

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.

• 농약과학회지
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• 제9권1호
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• pp.51-59
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• 2005

우리나라의 식품중 농약잔류허용기준 설정은 GAP에 의한 과학적인 자료, 농약 1일 섭취허용량(ADI), 식품섭취량, 평균체중 등을 기본으로 하여 설정된다. 농약잔류허용기준은 일반적으로 이론적인 농약섭취량(TMDI)은 ADI보다 낮게 설정된다. 연구결과를 보면, 104개 기준이 24개 농약에 대하여 새롭게 설정되며, 102개 기준이 이미 기준이 설정된 63개 농약에 추가 설정된다. 신규 농약중에 ethaboxam과 flupyra-zofos 농약의 유효성분은 우리나라에서 처음으로 개발되었다. 디치오카바메이트계 농약의 잔류허용기준은 디메칠디치오카바메이트(Dimethyldithiocarbamates), 에칠렌비스디치오카바메이트[Ethylenebis(dithiocarbamate)s] 및 프로피네브(Propineb) 3개 그룹으로 분류하여 신설하였다.

• 한국환경농학회지
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• 제42권1호
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• pp.71-81
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• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Fisheries and Aquatic Sciences
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• 제22권12호
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• pp.29.1-29.7
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• 2019

Veterinary drugs are widely used to protect production-related diseases and promote the growth of farmed fish. The use of large amounts of veterinary drugs may have potential risk and cause adverse effects on both humans and the environment. In this study, we developed risk-based ranking based on a scoring system to be applied in the national residue program. In this approach, the following three factors of veterinary drugs that may occur as residues in fishery products were considered: potency (acceptable daily intake), usage (number of dose and withdrawal period), and residue occurrence. The overall ranking score was calculated using the following equation: potency × usage (sum of the number of sales and withdrawal period) × residue occurrence. The veterinary drugs that were assigned high score by applying this approach were enrofloxacin, amoxicillin, oxolinic acid, erythromycin, and trimethoprim. The risk-based approach for monitoring veterinary drugs can provide a reliable inspection priority in fishery products. The developed ranking system can be applied in web-based systems and residuemonitoring programs and to ensure safe management of fishery products in Korea.

• 분석과학
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• 제18권3호
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• pp.250-256
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• 2005

고속액체크로마토그라피를 이용하여 동물성 식품 중 테트라싸이클린계 항생물질의 동시분석을 시도하였다. 대상물질은 동물의 질병치료.예방, 성장촉진 및 사료효율 개선에 널리 사용되는 클로르테트라싸이클린, 독시싸이클린, 옥시테트라싸이클린 및 테트라싸이클린이었으며, 대상식품은 쇠고기, 돼지고기, 닭고기, 우유, 계란, 넙치, 우럭, 참돔, 뱀장어 및 바다가재이었다. 시료를 McIlvaine 완충액 및 20% 삼염화초산으로 추출한 후 $C_18$ 카트리지로 정제하여 고속액체크로마토그라피로 분석하였다. 이동상으로는 0.01M 수산과 아세토니트릴의 혼합용액을 85:15에서 60:40까지 기울기로 사용하였으며 UV의 검출파장은 365 nm 이었다. 평균 회수율은 71-98% 이었으며, 검출한계는 신호대 잡음비 3 이상에서 클로르테트라싸이클린은 0.022, 독시싸이클린은 0.012, 옥시테트라싸이클린은 0.012 및 테트라싸이클린은 0.009 mg/kg이었다. 대부분의 시료에서 클로르테트라싸이클린, 독시싸이클린 및 테트라싸이클린은 검출되지 않았으나, 돼지고기, 넙치 및 참돔(2시료)에서 옥시테트라싸이클린이 각각 0.04, 0.17, 0.05 및 0.08 mg/kg로 모두 잔류허용기준을 초과하지 않은 수준으로 검출되었다.

• 한국축산식품학회지
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• 제38권5호
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• pp.1055-1063
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• 2018

The aim of study was to investigate the correlation between the level of 17 antibiotic residues and 6 antibiotic resistances of Escherichia coli isolates in chicken meats. A total of 58 chicken meats were collected from retail grocery stores in five provinces in Korea. The total detection rate of antibiotic residues was 45% (26 out of 58). Ten out of 17 antibiotics were detected in chicken meats. None of the antibiotics exceeded the maximum residue level (MRLs) in chicken established by the Ministry of Food and Drug Safety (MFDS). The most detected antibiotics were amoxicillin (15.5%), followed by enrofloxacin (12.1%) and sulfamethoxazole (10.3%). In a total of 58 chicken meats, 51 E. coli strains were isolated. E. coli isolates showed the highest resistance to ampicillin (75%), followed by tetracycline (69%), ciprofloxacin (65%), trimethoprim/sulfamethoxazole (41%), ceftiofur (22%), and amoxicillin/clavulanic acid (12%). The results of study showed basic information on relationship between antibiotic residue and resistance for 6 compounds in 13 chicken samples. Further investigation on the antibiotic resistance patterns of various bacteria species is needed to improve food safety.

• 한국식품과학회지
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• 제39권5호
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• pp.575-579
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• 2007

본 연구는 홍삼 및 농축액의 합리적인 농약잔류허용기준 개정을 위한 과학적인 자료를 얻고자 수행하였다. 인삼 재배 시에 사용 등록된 농약 3종(azoxystrobia, fenhexamid, cyprodinil)을 인삼포에 직접 살포하여 수확한 수삼을 홍삼과 농축액으로 직접 제조하였다. 수확한 수삼에 azoxystrobin 0.12 ppm, fenhexamid 0.19 ppm, cyprodinil 1.78 ppm이 잔류하였으며 농약이 잔류된 수삼을 원료로 홍삼 및 농축액으로 가공하여 각 제품의 농약 잔류량을 조사한 결과 fenhexamid의 경우 홍삼에 0.54 ppm, 홍삼농축액에서 1.93 ppm이 잔류하였다. Azoxysoobin은 홍삼에서 0.24 ppm, 홍삼농축액에서 0.81 ppm이 잔류하여 가공단계를 거치면서 증가하였다. 그러나 cyprodinil의 경우 1.78 ppm이 잔류된 수삼이 홍삼으로 가공되면서 1.49 ppm으로 감소하였으나 홍삼농축액에서는 3.66 ppm으로 증가하였다. 농약이 잔류된 수삼을 이용하여 홍삼과 농축액 제조시 azoxystrobin, fenhexamid, cyprodinil의 감소계수(dry base)는 홍삼에서 0.66, 0.94, 0.28, 홍삼농축액에서 3.25, 4.94, 1.01이였다.