• Title/Summary/Keyword: 잔류분 분석

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Development of the analytical method for pesticide residues in crops by using gas chromatograph / solvent free solid injector (GC / SFSI) (무용매 고체 시료 주입기(SFSI)를 이용한 작물 중 잔류농약의 기체크로마토그래피 분석법 개발)

  • Kim, M.R.;Lee, Y.;Park, B.J.;Choi, J.H.;Kim, I.S.;Shim, J.H.
    • The Korean Journal of Pesticide Science
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    • v.9 no.3
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    • pp.237-242
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    • 2005
  • This experiment was carried out to develop the fast and simple method for pesticide residue analysis by using solvent free solid injector (SFSI) and to validate the efficiency of the method developed for the residue analysis of the endocrine disruptor-like pesticides such as endosulfan, metribuzin, trifluralin and vinclozolin. The samples after freeze drying were sealed in glass capillary tubes and then introduced into the heated injector of gas chromatogaphy. The required pre-heating times were 1 min for endosulfan and trifluralin, 5 min for vinclozolin, and 10 min for metribuzin. The detection limits of endosulfan in chinese cabbages, metribuzin in lettuces, trifluralin in spinachs and vinclozolin in hot peppers were 0.05, 0.1, 0.05 and 0.05 ng, respectively and their recoveries were ranged from 74%, $98{\sim}107%$, $86{\sim}95%$ and $94{\sim}95%$, respectively. The detected level of metribuzine residue in field lettuce samples by using the SFSI was 0.6 ng/mg.

A Study on the Risk Assessment of Pesticide Residues of Agricultural to Ensure Military Food Safety (군 식품 안전성 확보를 위한 농산물 잔류농약 위해도 평가 연구)

  • Cho, Sung-Yong;Seo, Jun-Ho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.10
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    • pp.137-143
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    • 2020
  • To ensure safety of raw materials for military foods, hazard assessment and monitoring of residual pesticides was conducted on agricultural products consumed by 9 companies based in Gyeongin and Gangwon. Residual pesticides were analyzed for 142 different products, by applying the multi-species pesticide polycomponent analysis method. Of the 36 samples analyzed, residual pesticides were detected in 7 samples, representing a detection rate of 19.4%. One particular pesticide residue was detected in peanuts, green onions, and red pepper powder, and 20 types of pesticide residues were detected in red pepper powder used in combat foods. However, all residues were found to be below the permissible level. Moreover, the hazard assessment results for Cypermethrin, Tebuconazole and EPN showed the highest concentration among the residual pesticides detected. Since the estimated intake was less than 100% as compared to the ingestion limit, it was considered to be safe. I have suggested the edit as per my understanding. Please review for accuracy, and revise appropriately if required. This is the first pesticide Risk Assessment study encompassing military requirements. Considering the results, we expect further application research, including research on reducing hazardous materials.

The State-of-the-Art on Technologies for Treatment of Polychlorinated Biphenyls(PCBs) Pollutants (잔류성 유기오염물질 Polychlorinated Biphenyls(PCBs) 분해 처리 기술 현황)

  • Lee, Sang-Hoon;Sea, Bongkuk
    • Clean Technology
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    • v.11 no.1
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    • pp.29-39
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    • 2005
  • Polychlorinated biphenyls, (PCBs) are a group of highly toxic chlorinated industrial chemicals used as dielectrics, coolants and lubricants in electrical transformers. This article reviewed the state-of-the-art on technologies for decomposition of Polychlorinated biphenyls (PCBs), one of the persistent organic materials (POPs). The purpose of this study was to evaluate the feasibility of decontaminating PCBs contaminated pollutants using treatment technologies such as chemical dechlorination, photodegradation and biological transformation.

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Roughness Effect on the Residual Shear Characteristics of Jumunjin Sands (거칠기 효과를 고려한 주문진 표준사의 잔류전단강도 특성 분석)

  • Sueng-Won Jeong
    • The Journal of Engineering Geology
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    • v.33 no.4
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    • pp.717-724
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    • 2023
  • Residual shear strength is an important parameter in landslide dynamics and may be considered the critical factor in landslide triggering. Tests were undertaken using Jumunjin sands to examine the effects of smooth and rough surfaces on ring-shear characteristics. Under dense and drained conditions, shear velocities were recorded as 0.01, 0.1, 1, 10, 50, 100 mm s-1, with shear strength increasing with velocity and producing increasingly fine content. Particle fragmentation may thus increase landslide mobilization when the landslide body is mixed with ambient water in channelized flows.

Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

Determination of Amisulbrom Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.321-329
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    • 2014
  • This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

Residue of Combined Insecticide of Polynactin Complex(Tetranactin) and BPMC in Apple and Soil (Polynactin Complex (Tetranactin)와 BPMC 혼합제의 사과 및 토양 잔류성)

  • Yoon, Jae Cheon;Lee, Seok Joon;Park, Jong Woo;Kim, Jang Eok
    • Current Research on Agriculture and Life Sciences
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    • v.11
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    • pp.101-110
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    • 1993
  • The residues of combined insecticide of polynactin complex(tetranactin) and BPMC were determined to establish an index for the safety use to apple. Evaluation was made on residual concentration of tetranactin and BPMC in apple as a function of application frequency and date when the combined insecticide of tetranactin and BPMC was sprayed into apple. Their persistence in soil were also studied under the field and laboratory conditions. Recovery percentage from apple was ranged from 74.0 to 77.5 in tetranactin, 87.1 to 83.6 in BPMC, those from soil was 82.3 to 88.4 in tetranactin, 83.6 to 887.1 in BPMC. The minimum detectable limits of tetranactin and BPMC were 0.01ppm in apple pulp and 0.03ppm in apple peel and soil. The residue percentage of tetranactin and BPMC in the peel and pulp part of apple was about 96 in peel part by five sprays up to 3th day before harvest. The residues of tetranactin and BPMC in apple are proved to 0.39ppm and 0.75ppm by five sprays up to 30days before harvest. Maximum residue limit(MRL) of BPMC for fruits was established of 0.3ppm in Environment Protection Agency of Korea, and thus it is suggested that the preharvest intervals of combined insecticide for apple could be 30 days with twice spray. The half life of tetranactin in soil under field and laboratory conditions was 6.9 and 24.4 days, and in case of BPMC was 6.3 and 23.2 days, respectively.

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Residue Patterns and Biological Half-lives of Pyridalyl and Fluopicolide in Watermelon (수박 중 및 Pyridalyl 및 Fluopicolide의 잔류 특성 및 생물학적 반감기 산출)

  • Park, Ji-Su;Yang, Seung-Hyun;Choi, Hoon
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.50-56
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    • 2017
  • BACKGROUND: The present study was carried out to identify the residue patterns of insecticide pyridalyl and fungicide fluopicolide in watermelon and calculate the biological half-lives for establishing the pre-harvest residue limits (PHRLs). METHODSANDRESULTS:The watermelon samples for residue analysis were harvested 7 times during 0~10 days (Field 1) and 0~20 days (Field 2) after treatment of pesticides on watermelon in two different fields at the recommended dose, respectively. The residue analysis was conducted with HPLC/UVD. The method limit of quantitation (MLOQ) were set at 0.05 and 0.02 mg/kg, respectively, and overall mean recoveries were 81.2~90.5% for pyridalyl and fluopicolide. The residues in sample were stable for 43~47 days. The initial residue amount in field 1 and 2 were 0.12~0.16 mg/kg for pyridalyl and 0.23~0.24 mg/kg for fluopicolide, which were below maximum residue limit (MRL). The biological half-lives in field 1 and 2 were 26.9 and 17.9 days for pyridalyl and 16.6 and 94.2 days for fluopicolide, respectively. CONCLUSION: The PHRL for watermelon were estimated as 0.21 and 1.03 mg/kg for pyridalyl and flopicolide at 10 days before harvesting. The residue patterns of pyridalyl and fluopicolide were characterized by a very slow decrease of residue levels in watermelon.

HPLC를 이용한 축육(Pork Muscle)내의 Dihydrostreptomycin 검출법

  • Choe, Ji-Hyeon;Han, Eun-Yeong;Park, Jin-Gwan;Lee, Su-Yeon;Choe, Dong-Mi;Sin, Ho-Cheol;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.196-203
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    • 2005
  • 축산식품 고기내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발 을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/Dihydro streptomycin, Neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법 등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 DST에 대한 HPLC법에 대한 보고한 P. Edder 방법 중에 clean-up과정 및 이동상 조건을 대폭 수정하여 DST의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering Laboratories, Inc.)의 컬럼온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, reagent 유속 0.6ml/min mobile phase 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 DST 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 DST의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection (LOD)은 0.02ppm이었으며, 적어도 고기에서의 MRL이 0.6ppm임을 감안하면 DST를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 고기에 표준 DST를 1ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 DST의 limit of quantification(LOQ)는 약 0.47ppm이었으며, 이에 대한 회수율은 97.7%(n= 8)를 나타냈다. 실제 codex에서 권장한 고기의 MRL이 0.6ppm인 점을 감안하면 codex 권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발된 시험법은 지금까지 국내적으로 DST에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 DST에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 DST에 대한 분석시험법의 개발이 가능하다고 여겨진다.

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Residue Analysis of Quinclorac in Soil by Supercritical Fluid Extraction and Fluorogenic Derivatization Coupled with High Performance Liquid Chromatography (초임계추출과 형광유도체를 이용한 HPLC 에서의 Quinclorac 의 토양중 잔류분석)

  • Kim, Yong-Whan
    • Applied Biological Chemistry
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    • v.40 no.5
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    • pp.442-446
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    • 1997
  • A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.

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