• Title/Summary/Keyword: maximum residue limits

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Determination of Four Macrolide Antibiotics Residues in Chicken Muscle Using High-Performance Liquid Chromatography (액체크로마토그래피를 이용한 닭고기 시료에서의 마크로라이드계 동시분석법 개발)

  • Lee, Sang-Hee;Yoo, Miyoung;Shin, Dong-Bin
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.19-23
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    • 2013
  • A simple and rapid method has been developed and validated for simultaneous determination of each macrolides residues (spiramycin, josamycin, tilmicosin, tylosin) in chicken muscle by high-performance liquid chromatography- photo diode array (HPLC-PDA). Chicken muscle sample have been extracted with liquid-liquid extraction process; analytes was extracted by acetonitrile, and then defatted with hexane saturated by acetonitrile. The HPLC separation was performed on a Unison UK-$C_{18}$ ($150mm{\times}3.0mm$, $3{\mu}m$) with a gradient system of 0.1% trifloroacetic acid (TFA) and 0.1% trifloroacetic acid (TFA) in acetonitrile as the mobile phase. The drugs were detected at 232 nm for spiramycin and josamycin, and 287 nm for tilmicosin and tylosin. The limits of quantification (LOQs) were between 27 and $59{\mu}g/kg$; and the intra- and inter-day precision (relative standard deviation; RSD) was between 0.9-13.2 and 2.4-13.1%, respectively in chicken muscle sample. The method may has been successfully applied for multiresidue determination of four macrolides below the maximum residue limits (MRLs) established by the European Union (EU).

Analysis and Monitoring of Residues of Aminoglycoside Antibiotics in Livestock Products (축산식품 중 아미노글리코사이드계 항생제 잔류량 분석 및 실태조사)

  • Kang, Young-Woon;Joo, Hyun-Jin;Kim, Yang-Sun;Cho, Yu-Jin;Kim, Hee-Yun;Lee, Gwang-Ho;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.43 no.1
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    • pp.1-5
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    • 2011
  • It is possible that veterinary medicines remain in livestock food products, according to the use of many and various veterinary medicines to protect against disease when livestock animals are breed in limited space. Concentrated and continuous monitoring of residues is needed due to increases in resistance to antibiotics and side effects by eating livestock food products. We developed an analysis method for detecting streptomycin, dihydrostreptomycin, neomycin, gentamicin and spectinomycin in meat using LC/MS/MS and measured sensitivity, precision, accuracy, linearity and recovery according to CODEX guidelines to acquire confidence in the analysis method. Based on the results, we acquired good sensitivity compared to the maximum residue limit (MRL) as limits of detection (LOD) were 0.002-0.016 mg/kg and limits of quantification (LOQ) were 0.006-0.050 mg/kg. The analysis method satisfied the CODEX guidelines. The linearity ($r^2$) values of aminoglycoside antibiotics were 0.9936-0.9980, recoveries were 60-110% and relative standard deviations (RSD) were within 15%. As a result of monitoring for residues in a total 250 samples of livestock foods such as pork, chicken, and beef by the confirmed method, dihydrostreptomycin and gentamicin were detected in 5 pork samples. The residues of these antibiotics were within the MRLs. Thus, the detection ratio was 2% as 5 samples were identified from 250 samples.

Suggestion for Establishment of Temporary MRLs and Safe use Guideline of the Organophosphorus Insecticides in Jinpi (한약재 진피에 대한 유기인계 살충제의 잠정 MRL 설정 및 안전사용기준 제안)

  • Lee, Ju-Hee;Shin, Kab-Sik;Jeon, Young-Hwan;Kim, Hyo-Young;Hwang, Jeong-In;Lee, Byung-Hee;Kang, In-Hoo;Kang, Shin-Jung;Kim, Tae-Hwa;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.29 no.1
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    • pp.66-71
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    • 2010
  • Jinpi(Aurantii nobilis Pericarpium) is one of the most important material of oriental herbal medicine which is made from the peel of mandarin by washing with hot water and drying. Pesticides have necessarily used for mandarin cultivation according to their preharvest intervals (PHIs) but their maximum residue limits (MRLs) and PHIs for Jinpi are not established yet. This study is to know residue amount of organophosphorus insecticides in Jinpi and to establish the MRLs and PHIs for fenitrothion and phenthoate in Jinpi. Fenitrothion was sprayed once, twice and three times with 7 days interval before harvest. Its residue amount ranged from 0.14 to 1.17 mg/kg in mandarin, 0.59 to 4.02 mg/kg in its peel and 1.66 to 22.38 mg/kg in Jinpi. In case of phenthoate, it was sprayed with 10 days interval for 10 days before harvest. Its residue amounts in mandarin, its peel, and Jinpi ranged from 0.16 to 0.65, 0.69 to 2.41 and 1.69 to 11.3 mg/kg, repectively. Proposed MRLs of fenitrothion and phenthoate for Jinpi are suggested to 22.39 and 11.30 mg/kg, respectively. So we recommend PHIs of the pesticides that fenitrothion can be sprayed 3 times 7 days before harvest and in case of phenthoate, sprayed 3 times 10 days before harvest.

Determination of Residue Levels of Ethyl Carbamate in Alcoholic Beverages by Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS) (가스크로마토그래피/질량분석기(GC/MS/MS)를 이용한 주류 중 에틸카바메이트 잔류량 조사)

  • Kim, Dong-Ho;Jang, Han-Sub;Choi, Gu-Il;Kim, Hyun-Jung;Kim, Ho-Jin;Kim, Hyo-Lin;Kim, Keun-Sung
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.63-68
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    • 2013
  • Ethyl carbamate (EC) is a contaminant generated in the fermentation processes of various fermented foods. In this study, residue levels of EC in 95 alcoholic beverage samples were determined by using Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS). All the samples were purified by a liquid-liquid extraction (LLE) method using dichloromethane. The LLE method enables an improvement in time and cost to detection and specificity over the conventional extraction methods. The limits of detection and quantification (LOD and LOQ) to analyze EC were 1.3 and 4.0 ng/mL, respectively. The recovery rates of EC were ranged from 90.0 to 97.5% at the levels of 50, 100, and 500 ug/L. Among traditional grain-based alcoholic beverage samples (n = 34), the average residue levels of EC in takju, yakju, and cheongju were 0.63, 7.01, and 14.11 ug/L, respectively. Among fruit-based alcoholic beverage samples (n = 48), those of EC in japanese apricot spirits, bokbunjaju, grape wines, and other fruit wines were 79.18, 1.66, 2.64, and 2.39 ug/L, respectively. Among distilled or diluted alcoholic beverage samples (n = 13), those of EC in soju (distilled or diluted), general distillates, liquors, and brandies were 0, 3.30, 8.20, and 8.52 ug/L, respectively. Therefore, this study reports that the residue levels of EC in the alcoholic beverages, distributed in the current domestic markets, did not reach its maximum allowed levels of 30 and 400 ug/L established for grape and fruit wines in Canada, respectively.

Monitoring of Residual Pesticides in Commercial Agricultural Products in Korea (국내 유통 농산물의 농약 잔류실태 모니터링)

  • Kim, Hee-Yeon;Park, Hyoung-Joon;Lee, Jin-Ha;Gwak, In-Shin;Moon, Hyung-Sil;Song, Mi-Hye;Jang, Young-Mi;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Yoon, Sang-Hyeon
    • Korean Journal of Food Science and Technology
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    • v.39 no.3
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    • pp.237-245
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    • 2007
  • We tested for residual pesticide levels in agricultural products purchased from 5 provinces within the middle region of Korea during 2006. A Total of 488 samples of 23 different types of agricultural products were analyzed by GC/MS, GC-NPD, and LC/MS/MS. We used multi-analysis methods to analyze for 231 different pesticide types; a single residual pesticides were detected in 92 samples (18.9%), of which 9 samples (1.9%) exceeded the Korea Maximum Residue Limits (MRLs). we detected pesticide residue in more than 50% of the pepper leaf and welsh onion samples. For the welsh onions, 16 among the 30 analyzed samples contained pesticide residue, and 4 samples exceeded the Korea MRLs. Among the 234 kinds of pesticides we tested for, 42 were detected, and 21 of them were detected more than twice. Six pesticide residue types, including cypermethrin, iprodione, fludioxonil, ethoprophos, flutolanil, and lufenuron, exceeded the MRLs. No residual pesticides were detected in 396 of the samples (81.1%), and the residual pesticide levels in 83 samples (17.0%) were lower than the Korea MRLs, indicating that 98.1% of the samples were relatively safe.

Monitoring of pesticide residues in commercial agricultural products in the northern area of Seoul, Korea (서울 북부지역 유통 농산물의 농약 잔류실태)

  • Han, Sung-Hee;Park, Sung-Kyu;Kim, Ouk-Hee;Choi, Young-Hee;Seoung, Hyun-Jung;Lee, Young-Ju;Jung, Jung-Hee;Kim, Yun-Hee;Yu, In-Sil;Kim, Yoo-Kyung;Han, Ki-Young;Chae, Young-Zoo
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.109-120
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    • 2012
  • This study was conducted to monitor 284 pesticides residue level in 2,914 commercial agricultural products in the northern area of Seoul in 2011 by the multi class pesticide multiresidue analysis methods in Korea Food Code using GC, HPLC, GC-MSD and, LC-MSD. The detection rate of pesticide residues were 14.8% (431/2,914). The order of agricultural products in which the pesticide residues were detected was perilla leaves 40.0% (28/70), chamnamul 35.5% (11/31), amaranth 30.0% (3/10) and spinach 27.7% (38/137) etc. The percentage of products that exceeded the MRLs (maximum residue limits) were 1.0% (31/431). Those products that exceeded MRLs were ginseng (6), perilla leaves (4), leek (4), welsh onion (3) and sedeum (3) etc. The 59 kinds of the pesticides were detected on this study, 21 pesticides of them were detected over MRLs. Detection rate of fungicides (56.4%) was higher than that of insecticides (42.1%). And procymidone was detected with considerable high frequency. Additionally, residual residual violates pesticides were in the order of tolclofos-methyl, endosulfan, dimethomorph, diniconazole and fludioxonil. According to the agricultural marketing channels, detection and excess rate of them were monitored. Detection and excess rate of samples circulated in agricultural traditional market were highest. The estimated daily intakes (EDI) of the pesticides were compared to personal acceptable daily intakes (PADI) in order to risk assessment by food consumption. Diazinon in Korean cabbage showed the highest %ADI, 2.9901 and others showed below 3.0 %ADI. Overall, these results indicate that residue levels of pesticides detected were evaluated as safe.

Reduction Factors and Risk Assessment of Organophosphorus Pesticides in Korean Foods (국내 식품 중 유기인계 잔류농약의 위해성 평가)

  • Lee, Mi-Gyung;Lee, Su-Rae
    • Korean Journal of Food Science and Technology
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    • v.29 no.2
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    • pp.240-248
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    • 1997
  • References on the cooking and processing losses of organophosphorus (OP) pesticides in foods were collected and analyzed to indicate that the average removal of whole pesticides being 45% in water washing, 56% in detergent washing, 91% in peeling of fruits, 5l% in blanching-boiling of vegetables, 90% in milling and processing of grains. The theoretical maximum daily intake (TMDI) calculated from the food intake and Korea maximum residue limits showed that 4 among 11 pesticides exceeded the acceptable daily intake (ADI). The estimated daily intake (EDI) calculated from the food intake and monitoring data reached 17.2% of ADI on the assumption that the toxicity of OP pesticides appears as an additive effect. The % ratio of ADI for individual pesticides was 6.1% in diazinon, 5.8% in fenthion, 3.3% in fenitrothion and very low in other pesticides. By applying reduction factors to the EDI, the removal ratio of OP pesticides in cooking and processing appears to be over 50%. In summary, the exposure level of Korean population toward whole OP pesticides was estimated to reach 23% of ADI, which would not cause any health rick as yet, but calls for a systematic risk assessment.

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Management of Veterinary Drug Residues in Food (식품 중 잔류동물용의약품의 안전관리)

  • Oh, Jae-Ho;Kwon, Chan-Hyeok;Jeon, Jong-Sup;Choi, Dong-Mi
    • Korean Journal of Environmental Agriculture
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    • v.28 no.3
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    • pp.310-325
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    • 2009
  • Veterinary drugs have been used to prevent livestock diseases for many years. In spite of having advantages, sometimes indiscriminate application, overdose and abuse may cause risk for human. Therefore, management and risk assessment of veterinary drugs become essential to ensure food safety. So the National Veterinary Research & Quarantine Service (NVRQS) impose on registration for use of veterinary drugs also Korea Food and Drug Administration (KFDA) fixed the maximum residue limits (MRLs) for veterinary drugs in food. Basically, KFDA set MRLs based on the veterinary drugs residual data. Moreover, KFDA estimates the theoretical maximum daily intake (TMDI) with food consumption data and population mean body weight. Recently, 116 veterinary drug MRLs including banned veterinary drugs have been established and other 32 veterinary drugs MRLs will be established within 2009. In 2010, MRLs among antibiotics and synthetic antibacterial agents in livestock fishery products (including milk and eggs) and honey (including royal jelly and propolis) which have not been set in Korea Food Code and Codex Alimentarius Commission (CAC) will be regulated as uniform limit (0.03 mg/kg). In future, veterinary drugs will be controlled strictly to strengthen public health by improving analytical method.

An Impact Assessment on Atmospheric Dispersion of Pesticide using AGDISP Model (AGDISP모델을 이용한 농약의 대기확산 영향평가)

  • Kim, Jeong-Hwan;Koo, Youn-Seo;Lee, Seung-Hoon
    • Journal of Environmental Impact Assessment
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    • v.22 no.6
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    • pp.547-556
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    • 2013
  • Recently, golf courses have increased over the years because golf became popular leisure sport. Various environmental problems have been then issued by a golf course during constructing and running them. A problem of pesticide, which is serious among various environmental problems, from golf course has harmful effect on surrounding area and makes human suffer from acute and chronic diseases. Pesticides are used for the cost-effective managing of golf course and the amount of pesticides also increases as the number of golf course increase. Since the assessment of pesticides on near-by surrounding has been focused on water and soil media, studies related to atmospheric dispersion have been hardly attempted. The method to assess an impact of pesticide nearby agricultural production by the atmospheric dispersion using AGDISP(AGricultural DISPersal) model was developed and applied to the actual planned golf course located in Hongcheon, Gangwon. For implementing AGDISP, parameters were investigated from the golf course's land use planning map, pesticide spray device, Hong-Cheon weather station and etc. First of all, a kind of pesticide, a form of spraying pesticide, geographical features, weather data, and distance(golf course to plantation) were investigated to understand how to work these parameters in AGDISP. Restricted data(slope angle, droplet size distribution and solar insolation) sensitivity analysis of these parameters to estimate effect of pesticide nearby a plantation and a high relative contribution data of analyzed data was selected for input data. Ethoprophos was chosen as the pesticide used in the golf course and the amounts of pesticide deposition per annual agricultural productions were predicted. The results show that maximum amount of pesticide deposition through atmospheric dispersion was predicted $2.32{\mu}/m^2$ at 96 m where the nearest organic plantation exists. The residues of pesticide were also estimated based on the annul production of the organic and the deposition amount of the pesticide. Consequently, buckwheat, wheat and millet were likely to exceed maximum residue limits for pesticides in foods(MRL) and sorghum, corn and peanut were likely to exceed MRL by organic farming as well.

Monitoring of pesticide residues in peppers from farmgate and pepper powder from wholesale market in Chungbuk area and their risk assessment (충북지역 산지 고추와 유통 고춧가루 중 잔류농약 모니터링 및 위해성 평가)

  • Kim, Kwang-Ill;Kim, Heung-Tae;Kyung, Kee-Sung;Jin, Chung-Woo;Jeong, Chan-Hee;Ahn, Myung-Soo;Sim, Seok-Won;Yun, Sang-Soon;Kim, Yun-Jeong;Lee, Kwang-Goo;Lee, Kee-Doo;Lee, Won-Jae;Lim, Jeong-Bin
    • The Korean Journal of Pesticide Science
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    • v.10 no.1
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    • pp.15-21
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    • 2006
  • In order to monitor the pesticide residues in/on peppers and pepper powder and to assess their risk, pesticides in/on green pepper from 10 farmgates and fresh red pepper from 9 farmgates in Chungbuk area and pepper powder from 6 wholesale markets in Cheongju city were analyzed with a GLC and an HPLC. Also, pepper powder made by pulverization of the dried red pepper was analyzed to elucidate the change of pesticide residues in fresh red pepper by oven-drying. The number of pesticides detected from peen pepper, fresh red pepper, dried red pepper and pepper powder were 9, 12, 12, and 17, respectively, including 10 pesticides (one fungicide and nine insecticides) which were exceeded the maximum residue limits (MRLs). The exceeding rate of the MRL were higher in dried red pepper and pepper powder than in green pepper and fresh red pepper. Although some pesticides in peppers and pepper powder exceeded the MRLs, their estimated daily intake(EDI) were less than 1.6% of their acceptable daily intakes(ADIs), suggesting that it would be estimated to safe. By oven-drying of fresh red pepper at $65^{\circ}C$ for 72 hours, the weight of dried red pepper was from 1/5.9 from 1/7.8 of fresh red pepper, while the concentration of pesticide residue in dried red pepper increased from 1.7 to 8.2 times, suggesting that further reconsideration was required for the MRL of pepper powder.