• Title/Summary/Keyword: Residue Limit

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Simultaneous Determination of Residual Sulfonamides in Meat Tissues by High Performance Liquid Chromatography (HPLC에 의한 식육조직중의 잔류 설파제 동시 분석)

  • 강희곤
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.37-42
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    • 1994
  • Four sulfoanmides ; sulfamerazine ; sulfamethazine, sulfathiazole and sulfadimethoxine from muscle, kindney, liver and heart tissues of pork and chicken by LC. Residual sulfonamides were extracted with dichloromethane and determined on a Sperisorb ODS-1 column(250mm$\times$4.6mm id) with acetonitrile/water/acetic acid (30/70/0.3 v/v) as a mobile phase at 260nm. Recoveries from 4 tissues of pork and chicken samples fortified with 50 and 100 ppb were 71.2~87.2% and 73.7~89.6%, respectively. The detection limit was 0.03 $\mu\textrm{g}$/g in each drug. Sulfamethazine in 5 samples of pork. And sulfadimethoxine in 5 samples and sulfamethazine in 3 samples were also detected from 41 samples of chicken. The order of residue levels of sulfonamides in tissues was kidney>liver>heart>muscle, respectively. The residue levels of sulfonamides from kidney and liver were 0.03~0.15 $\mu\textrm{g}$/g in porks and 0.03~0.10 $\mu\textrm{g}$/g in chickens.

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Development of Multi-Residue Methods for Carbamate Pesticides by the Enzyme Inhibition Test (효소 저해법을 이용한 Carbamate계 농약의 다성분 잔류분석법 개발)

  • Kim, Jung-Ho
    • Journal of Environmental Science International
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    • v.17 no.12
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    • pp.1325-1330
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    • 2008
  • This study was carried out with the detection for multiresidue of the carbamate pesticide such as carbaryl and cabofuran by enzyme-inhibition method. The check time for determination of acetylcholinesterase(AChE) activity was selected at 60 sec. The AChE activity in chicken brain determined by the Ellman's method was $162{\mu}$mol/min/g protein. $I_{50}$ for AChE by carbamate pesticide with wet kit was 0.169mg/L of carbaryl and 0.089mg/L of cabofuran, respectively. The incubation time for enzyme kit with substrate kit was 30min for determination of AChE activity. Enzyme kit with substrate kit was stable at $4^{\circ}C\;and\;25^{\circ}C$ for 5 days. Limit detection concentration of carbaryl with dry kit for AChE was 0.05mg/L. The dry kit such as wet kit applied Enzyme-Inhibition(EI) method with AChE was confirmed the multi residue method to detect the carbamate pesticides.

Determination of tetracycline antibiotics in food (식품 중 테트라싸이클린계 항생물질의 분석)

  • Park, Dongmi;Jeong, Jiyoon;Chang, Moonik;Im, Moohyeog;Park, Kunsang;Hong, Mooki
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.250-256
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    • 2005
  • A selective method of high performance liquid chromatography with UV detector has been applied to determine 4 tetracycline antibiotics in the animal food, simultaneously. The targets were chlortetracycline (CTC), doxycycline (DC), oxytetracycline (OTC), and tetracycline (TC) that are used routinely in veterinary medicine for prevention and control of disease. Food samples were beef, pork, chicken, milk, whole egg, flatfish (Limanda yokohamae), jacopever (Sebastes hubbsi), seabream (Chrysophrys major), eel (Anguilla japonica) and lobster (Hommarus americanus). After extracting food samples with 20% trichloroacetic acid and McIlvaine buffer, they were purified by a $C_18$ SPE cartridge with 0.01M methanolic oxalic acid solution. The concentrated residue was re-dissolved in methanol, filtered, cleaned up and analyzed on a $C_18$ column. The mobile phase was a mixture of 0.01M oxalic acid and acetonitrile with a gradient ratio from 85:15 to 60:40. The UV wavelength was 365 nm. The overall recoveries were ranged from 71% to 98% and the limit of detections were 0.022 for CTC, 0.012 for DC and OTC and 0.009 mg/kg for TC at signal/noise > 3, respectively. As results, CTC, DC and TC were not detected in all selected food samples, however, OTC was detected in meat and fishes. The determined level of OTC was 0.04 ppm for pork, 0.17 ppm for flatfish and 0.05 and 0.08 ppm for jacopever, that were within the Maximum Residue Limits (MRLs) in the food.

Changes in Phytoavailability of Heavy Metals by Application of Limestone in the Farmland Soil nearby Abandoned Metal Mine and the Accumulation of Heavy Metals in Crops (폐금속 광산 주변 농경지 토양에서 석회석 처리에 의한 중금속의 식물유효도 변화 및 작물의 중금속 축적)

  • Yun, Sung-Wook;Yu, Chan
    • Journal of The Korean Society of Agricultural Engineers
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    • v.54 no.3
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    • pp.1-9
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    • 2012
  • As topographic characteristics of Korea where 64 % of the national land area is forest and only 17 % is being used as farmland, remediation of farmland contaminated by heavy metals is a considerably important issue. In this study, as an alternative of practically and effectively remediating farmland which was abandoned as its crop plants exceeded maximum residue limit of heavy metals due to mining impact, applicability of stabilization method was examined through the pilot-scale field experiment. Three plots ($L{\times}W{\times}D=3m{\times}2m{\times}0.3m$) were installed at the selected farmland and in plot 1, only soil of the selected farmland was applied, in pilot 2, soil of the selected farmland plus 3 % limestone (w/w) was applied and in pilot 3, soil of the selected farmland plus 3 % limestone was applied and then uncontaminated soil was covered thereon (0.3 m). After that, seeds of radish, Korean cabbage and soybean of which characteristics of edible portions are different were sowed on each plot and cultivated. Afterwards, at a proper harvesting time (app. 80 days later), crop plants and soil were collected and phytoavailability (0.11 M HOAc extractable) of heavy metals in soil and accumulated concentration of heavy metal in edible portion of crop plants were examined. As a result, it was revealed that phytoavailability of heavy metals in soil added with limestone (plot 2) was clearly reduced compared with plot 1 (untreated) and owing to this treatment, accumulated concentration of heavy metals in edible portion of crops was also clearly reduced compared with plot 1. While radish cultivated in plot 1 had exceeded maximum residue limit of agricultural products, in particular, plot 2 using limestone had shown concentration lower than maximum residue limit and this plot had shown little difference with 3 plot where crop was cultivated in uncontaminated soil cover. Therefore, it was considered that for abandoned farmland like the selected farmland, reducing mobility and phytoavailability of heavy metals and reducing crop uptake through stabilization method would be an effective and practical alternative for producing safe agricultural products on a sustained basis.

Establishment of Pre-Harvest Residue Limits and Residue Characteristics of Penthiopyrad and Pyriofenone in Cucumber (Cucumis sativus L.) Under Greenhouse Condition (시설 내 오이(Cucumis sativus L.) Penthiopyrad 재배 중 및 Pyriofenone의 잔류특성과 생산단계 잔류허용기준 설정)

  • Leem, Su-Bin;Kim, Ji-Yoon;Hur, Kyung-Jin;Kim, Hee-Gon;Hur, Jang-Hyun
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.43-49
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    • 2017
  • BACKGROUND: Greenhouse crops are one of agricultural products consumed largely in Korea. Cucumber is a typical example as main vegetables of greenhouse crops. Thus, pesticide residue analysis is an important requirement to guarantee pesticide safety of cucumber. This work was aim to investigate the residues of penthiopyrad and pyriofenone in cucumber after harvest. METHODS AND RESULTS: Cucumber was subjected to treat with penthiopyrad and pyriofenone at a level of recommended dose 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The samples were extracted with organic solvent by using a homogenizer and purified on solid phase cartridge column followed by LC-MS/MS analysis. The recovery levels of penthiopyrad and pyriofenoneranged from approximately 81 to 93% with the method limit of 0.005 mg/kg and coefficient of variation less than 10%. Penthiopyrad and pyriofenone were detected at a level less than maximum residue limit in cucumber at 10 days before. The half-lives of penthiopyrad and pyriofenone were determined to 2.4 ~ 2.6 days. CONCLUSION: Penthiopyrad and pyriofenone are suggested to use in cucumber 10 days before harvest to reach their levels less than maximum residue limit.

Assessment of the Residues of Benfuresate and Oxolinic Acid in Crops (Benfuresate와 Oxolinic Acid의 작물체중 잔류량 평가)

  • Park, Dong-Sik;Yang, Jae-E.;Han, Dae-Sung
    • Korean Journal of Environmental Agriculture
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    • v.14 no.3
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    • pp.312-318
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    • 1995
  • Residues of benfuresate in rice and oxolinic acid in Chinese cabbage were determined through the field experiments in order to establish the safe use and the maximum residue limit(MRL) of these pesticides in Korea. The herbicide benfuresate powder was sprayed into the paddy field with a level of 0.6kg(active ingredient)/ha and rice (Oryza sativa L.) was grown. At harvest, residues of benfuresate in brown rice and stem were analyzed using gas chromatograph. The residue of oxolinic acid in Chinese cabbage (Brassica campestris subsp. napus var pekinesis MAKINO) was analyzed using HPLC after foliar-spraying this fungicide into the cabbages at a level of 15kg/ha. The recovery efficiencies of benfuresate and oxolinic acid were 87-89% and 90-95%, respectively. The respective residues of benfuresate in rice and oxolinic acid in Chinese cabbage were in the range of 0.27-0.46 mg/kg and 0.23-1.53kg/kg. Residual concentrations of these pesticides in crops increased with the increased application frequencies, followed the first-order kinetics and linearly decreased with time. The highest residue of 1.53 mg/kg of oxolinic acid was observed when this fungicide was sprayed six times until three days prior to harvest, but this level was far lower t㏊n 5 mg/kg, which is the maximum residue limit(MRL) set by FAO/WHO.

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Residue Analysis to Establish an Index for the Safety Use of Propineb (Propineb의 안전사용(安全使用) 기준(基準) 설정(設定)을 위한 잔류분석(殘留分析))

  • Choi, Won-Seog;Yang, Jae-Eui;Han, Dae-Sung
    • Korean Journal of Environmental Agriculture
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    • v.11 no.3
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    • pp.209-214
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    • 1992
  • Residue of Propineb in Sesame(Sesamum indicum L.) seed was determined to establish an index for the safety use of Propineb to Sesame. Evaluation was made on residual concentration of Propineb in Sesame seed as a function of application frequency and date when the mixed formulations of Propineb(56%), protectant fungicide, and Oxadixyl(8%), contact fungicide, were sprayed into Sesame leaves. Level of Propineb treatment was $0.028g/m^2$ with various combinations of application time from three to sixty days before harvest. Results are summarized as followings. 1. Recovery percentages of Propineb from Sesame seed were ranged from 84 to 96, and the minimum detectable limit of Propineb with the method employed in this experiment was 0.03mg/kg. 2. Residues of Propineb in Sesame seed were in the ranges of 0.14 to 1.38mg/kg, varying with frequency and date of Propineb application. 3. Residues of Propineb increased as increasing application frequency of Propineb or as being application date closer to harvest time. 4. Residue of Propineb in Sesame seed was decreased with time, showing to be fitted to the first-order kinetics. 5. Residues of Propineb in Sesame seen were, irresepective of treatments, lower than 2mg/kg, the Maximum Residue Limit(MRL) established by FAO/WHO. 6. Half-life of Propineb determined in this experiment was ranged from 12 to 16 days.

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Establishment of the Korean total diet study (TDS) model in consideration to pesticide intake (한국형 총식이섭취조사(Total Diet Study, TDS) 모델 확립을 위한 농약섭취수준에 대한 접근)

  • Yang, An-Gel;Shim, Ki-Hoon;Choi, Ok-Ja;Park, Jong-Hyouk;Do, Jung-Ah;Oh, Jae-Ho;Hwang, In Gyun;Shim, Jae-Han
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.151-162
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    • 2012
  • This study was carried out to establish Korean total diet study (TDS) model for estimating pesticide residue in food samples. In addition, pesticide residues of food samples were monitored by setting the standards of established Korean total diet study model. For monitoring, first step were selection of total 102 species food samples, second step were selection of total 70 species food samples, and third step were selection of total 12 representative diet and 109 species food samples. Ninety-eight pesticides were analyzed using $GC-{\mu}ECD$, GC-MS, and LC-MS/MS after QuEChERS sample preparation method. The residue levels in detected food samples were below the maximum residue limit (MRL). Establishment of the Korean total diet study model means providing safe food for consumers, secure the safety of food samples and provide ongoing information to agricultural producers about use of pesticides.

Effects of Treatment Time of Cadusafos and Fosthiazate for the Control of Meloidogyne arenaria on Oriental Melon (카두사포스와 포스치아제이트 처리시기에 따른 땅콩뿌리혹선충 방제효과)

  • 김동근;김진배;이재국;최성국;윤재탁
    • Korean journal of applied entomology
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    • v.41 no.4
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    • pp.293-298
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    • 2002
  • Cadusafos and fosthiazate were applied at the rate of 1.8 g a.i./6$\m^2$ as pre-plant or pre-plant+post-plant treatments on winter-grown oriental melon in a greenhouse soil infested with Meloidogyne arenaria. Nematicides reduced root-knot nematode population from 35 to 90% compared with control; fosthiazate was better than cadusafos (P = 0.003) and fosthiazate pre-plant+post-plant application reduced nematode population densities as much as 90%. Nematicides increased yield in an average of 23% (11-38%) in May, 39% (2-65%) in June, and 31% (12-46%) for the total (P = 0.085). The residue in the fruit of oriental melon by post-plant treatment of fosthiazate exceeded maximum residue limit of 0.2ppm, while the Cadusafos residue was below the limit. It is concluded that fosthiazate cannot be used as a post-plant treatment in winer-grown oriental melon with overall consideration, i. e., danger of residue, value of melon, costs of nematicide, consumer demand on safer agricultural products, and effects of fallow.

Residual characteristics of insecticide flubendiamide in kale (케일 중 살충제 Flubendiamide의 잔류 특성)

  • Kim, Hyun-Jin;Hwang, Kyu-Won;Sun, Jung-Hun;Lee, Tae-Hyun;Jeong, Kyoung-Su;Moon, Joon-Kwan
    • Journal of Applied Biological Chemistry
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    • v.65 no.3
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    • pp.173-181
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    • 2022
  • This study was carried out to investigate the residual characteristics of flubendiamide in kale to establish pre-harvest residue limits (PHRL) and the removal efficiency according to the washing solvent and method. Field tests were conducted at two different greenhouses, field 1 (Anseong-si, Gyeonggi-do) and field 2 (Incheon-si, Gyeonggi-do). According to the safe use guidelines kale was sprayed with flubendiamide twice every 10 days and harvested 0 (after 2 h), 1, 2, 3, 5, 7 and 10 days after the final application. The biological half-live of flubendiamide in kale was calculated based on dissipation curves of the pesticide in samples analyzed by liquid chromatography coupled with tandem mass spectrometry. In the analysis, method limits of quantitation (MLOQ) were 0.01 mg/kg, and recoveries performed with two different fortification levels of 10 MLOQ and maximum residue limit (0.7 mg/kg) were 104.2±3.6 and 101.9±10.2%, respectively. The dissipation rate constant of flubendiamide in kales were 0.2437 at field 1 and 0.1981 at field 2. PHRL calculation equations obtained using the dissipation constants estimated as follows: if the residual concentration of flubendiamide in kale on 10 days before harvest is less than 8.0 mg/kg, the residual concentration on the harvest would be under MRL. The removal of flubendiamide from kale was the greatest when it was washed with vinegar (39.8%), followed by baking soda (31.7%), calcium powder (30.2%), neutral detergent (27.2%), and tap water (15.9%). The results of this study would be useful for both farmers and consumers to produce or consume safe agricultural products.