• Title/Summary/Keyword: drug residues

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High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Uncertainty Evaluation of the Analysis of Methamphetamine and Amphetamine in Human Hair by GC/MS (GC/MS를 이용한 모발 중 메스암페타민 및 암페타민 분석의 측정불확도 평가)

  • Kim, Jin-Young;Kim, Jong-Sang;Kim, Min-Kyoung;Lee, Jae-Il;Suh, Yong-Jun;In, Moon-kyo
    • YAKHAK HOEJI
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    • v.51 no.3
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    • pp.206-213
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    • 2007
  • Recently estimating the uncertainty of an analytical result has become an essential part of quantitative analysis. This study describes the uncertainty of the measurement for the determination of methamphetamine and its major metabolite amphetamine in human hair, The method consists of washing, drying, weighing, incubation and extraction with methanolic HCI solution, clean-up, trifluoroacetyl derivatization, and qualification/quantification of residues by gas chromatography/mass spectrometry (GC/MS). Traceability of measurement was established through traceable standards and calibrated volumetric equipment and measuring instruments. Measurement uncertainty associated with each analyte in real samples was estimated using quality control (QC) data. The main source of combined standard uncertainty comprised two components, which are uncertainties associated with calibration linearity and variations in QC, while those associated with preparation of analytical standards and sample weighing were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method ranged for individual analytes from 4.99 to5.03%.

Development of Baccillus megaterium Disk Assay Kit for the Determination of Antibacterial Residues in Animal Tissues (식육중 잔류 향균물질의 검출을 위한 Bacillus megaterium 디스크 검사킷트 개발)

  • 손성완;조병훈;진남섭;이혜숙;윤순학;김재학;이재진;이영순
    • Journal of Food Hygiene and Safety
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    • v.11 no.4
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    • pp.315-321
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    • 1996
  • Various antimicrobial drug screen tests have been used in order to ensure food safety. However, the conventional screen tests, the Swab Test on Premises(STOP, USA), the Calf Antibiotic and Sulfa Test(CAST, USA) and the European Economic Community 4-plate Test(FPT, EU) are not sufficiently rapid or sensitive enough to detect low levels of sulfa drugs in meat. We developed a new screen test kit for the determination of the antimicrobial residues in meat called the Bacillus megaterium Disk Assay(BmDA). A comparison of BmDA with the older screen tests showed BmDA was as good as the older ones with several advantages. The new test kit is faster-it can be read in 4∼6 hours instead of 16∼18 hours. Moreover, BmDA can discriminate sulfa drugs from other antimicrobial drugs because p-aminobenzoic acid countacts the inhibiting action of sulfa drugs. Minimum detectable levels of sulfa drugs were significantly improved at the lever of 0.025*0.1 pp, compared with the level of 1.0 ppm in FPT. A comparison of BmDA with the older screen tests in HPLC confirmed meat samples exceeded the Korean tolerance value of 0.1 ppm showed BmDA was the most sensitive in the microbiological screen tests. As the microbiological screen tests have already known, a person familiar with simple laboratory techniques should have no difficulty in using it to detect antimicrobial residues in meat. This would be a simple, economic method of antimicrobial residues detection which might be succesfully used by many laboratories.

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The analysis of Residual Pesticides and Sulfur Dioxide in Commercial Medicinal Plants (유통 한약재의 잔류농약 및 잔류이산화황의 함량 분석)

  • Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyung
    • The Korea Journal of Herbology
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    • v.27 no.6
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    • pp.43-48
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    • 2012
  • Objectives : This study was investigated to determine the contents of pesticide residues and sulfur dioxide residues in commercial herbal medicines in Korea. Methods : Chromatographic test was performed on 100 samples consisted with 10 kinds of medicinal plants including improted and domestic products. To establish 19 pesticide residues (DDE, DDD, DDT, Dieldrin, Methoxychlor, BHC isomers, Aldrin, Endosulfan isomers, Endrin, Captan, Procymidone, Chlorpyrifos and Imidacloprid) in commercial herbal medicines, chromatographic equipments were used with the gas chromatography-mass detector and gas chromatography-electron capture detector for qualitative analysis. The imidacloprid analysis was performed by high performance liquid chromatograpgy-ultraviolet detector at 270 nm UV wavelength. The contents of sulfur dioxides were analyzed by modified Monnier-Williams method. All methods were based on notification procedure of Korea Food & Drug Administration (KFDA). Results : The residual pesticides were not founded in improted and domestic samples. Among 100 samples, the residues of sulfur dioxide in 73 samples were not detected and 25 samples showed contents in the range of 0~21.90 mg/kg. The excess samples of MRLs were 2 samples (30 mg/kg to medicinal herbs), Asiasari Radix et Rhizoma (Imported product) and the average amount of sulfur dioxide in 2 unsuitable samples were 14.83 mg/kg. These samples were found to transgress KFDA regulatory guidance of residual sulfur dioxide. Conclusion : These results are able to use as basic data to improve the reliability and value of commercial medicinal herbs.

Diseases of Aquaculture Animals and Prevention of Drug Residues (양식어류의 질병과 수산동물용 의약품의 잔류방지 대책)

  • Heo, Gang-Joon;Shin, Kwang-Soon;Lee, Mun-Han
    • Proceedings of the Korean Society of Food Hygiene and Safety Conference
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    • 1992.07a
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    • pp.7-19
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    • 1992
  • Fish pathology is one of the main scientific bases upon which this expansion in aquaculture has been dependent and requires a wide knowledge of the environmental constraints, the physiology and characteristics of the various pathogens, the responses of the host and the methods by which they may be controlled. The primary disease and parasite problems in aquaculture animals relate to viral, bacterial, fungal and protozoan epizootics. Parasitic nematodes, trematodes and cestodes are commonly found in aquaculture animals, but seldom are they present in concentrations sufficinet to cause significant problems. When an epizootic does occur and chemical treatment is indicated, the appropriate chemical must be selected and properly applied. We have antibiotics, sulfa, nitrofuran and other chemicals for treatment of fish diseases. Some may be mixed with the fred during formulation, added to the pellets of feed as a surface coating, given in the dorm of an injection or used as a bath. Even though a drug or chemical has been officially approved for use in aquaculture, the substance should never be used unless there is a clear need. Some of the reasions for this view are as follows: (1) the constant use of antibiotics can lead to the development of resistant strains of bacteria, (2) biofilter efficiency may be impaired or destroyed by chemicals added to closed recirculating water systems, and (3) the injudicious use of chemicals can have a damaging effect on the environment as well as on human.

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Residues of Heavy Metals and Organochlorine Pesticides in Ginseng at Environment of North Gyeongbuk (경북북부 인삼 재배환경 중 중금속과 유기염소계 농약의 잔류)

  • Park, Soo-Woon;Kim, Jung-Ho
    • Journal of Environmental Science International
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    • v.19 no.10
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    • pp.1203-1210
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    • 2010
  • To obtain the risk assessment of hazardous materials in ginseng, the residues of heavy metals and organochlorine pesticides in samples on the Yeungju and Sangju are surveyed. Cd and Hg in ginseng on Yeungju and Sangju is not detected. 0.21 mg/kg of As, 0.39 mg/kg of Cr, 0.14 mg/kg of Pb, 1.83 mg/kg of Cu, 3.93 mg/kg of Zn and 0.43 mg/kg of Ni in ginseng on Sangju are shown. 0.25 mg/kg of Cr, 0.08 mg/kg of Pb, 1.11 mg/kg of Cu, 8.99 mg/kg of Zn and 1.15 mg/kg of Ni in ginseng on Yeungju are detected. As and Pb in ginseng on Sangju are 7.0% and 2.8% for Korea Food & Drug Administration(KFDA) advisory level, respectively. Pb in ginseng on Yeongju are 1.6% for Korea Food & Drug Administration(KFDA) advisory level. The heavy metals such as AS, Cr, Cd, Pb, Cu, Zn, Hg, Ni in soil on Yeongju and Sangju are range of 0-20% for with Korea Food & Drug Administration (KFDA) level. BHC isomer, DDT isomer and endosulfan isomer are not detected in ginseng and soil on Yeongju and Sangju, respectively. Finally, the assessment of hazardous materials of the heavy metals and organochlorine pesticides in ginseng on the Youngju and Sangju are verified the safety the level compare with tolerances level for Korea.

Simultaneous Determination of Plasticizers in Food Simulants Using GC/MS

  • Park, Na-Young;Yoon, Hae-Jung;Kwak, In-Shin;Jeon, Dae-Hoon;Choi, Hyun-Chul;Eum, Mi-Ok;Kim, Hyung-Il;Sung, Jun-Hyun;Kim, So-Hee;Lee, Young-Ja
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.15 no.3
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    • pp.93-98
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    • 2009
  • Migration levels of plasticizers, di-n-butyl phthalate (DBP), benzyl-butyl phthalate (BBP), di-n-octyl phthalate(DNOP), di-iso-decyl phthalate (DIDP) and di-iso-nonyl phthalate (DINP), di-(2-ethylhexyl) adipate (DEHA), from 46 poly(vinyl chloride) (PVC) wrap films and 54 PVC gaskets into food simulants were determined using gas chromatography/mass spectrometry (GC/MS). The method was validated with limit of detection (LOD) of $0.01{\sim}0.02\;{\mu}g/mL$ for DBP, BBP, DNOP and DEHA, and $2\;{\mu}g/mL$ for DIDP and DINP. The linearity were found to be > 0.99 for all the compounds in concentration range of $0.1{\sim}81.4\;{\mu}g/mL$, and overall recoveries were ranged from 90.4 ~ 99.6%. DBP, BBP, DNOP, DEHA, DIDP and DINP were not detected in food simulants, except 1 wrap sample from which 0.28 and $0.99\;{\mu}g/mL$ of DEHA were detected respectively when tested with 20% ethanol and n-heptane as food simulants. These values were below the regulatory limitation in European Union (EU).

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Computational Analysis of Human Chemokine Receptor Type 6

  • Sridharan, Sindhiya;Saifullah, Ayesha Zainab;Nagarajan, Santhosh Kumar;Madhavan, Thirumurthy
    • Journal of Integrative Natural Science
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    • v.11 no.2
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    • pp.121-129
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    • 2018
  • CXCR6 is a major target in drug design as it is a determinant receptor in many diseases like AIDS, Type I Diabetes, some cancer types, atherosclerosis, tumor formation, liver disease and steatohepatitis. In this study, we propose the active site residues of CXCR6 molecule. We employed homology modelling and molecular docking approach to generate the 3D structure for CXCR6 and to explore its interaction between the antagonists and agonists. 3D models were generated using 14 different templates having high sequence identity with CXCR6. Surflex docking studies using pyridine and pyrimidine derivatives enabled the analysis of the binding site and finding of the important residues involved in binding. 3D structure of CXCL16, a natural ligand for CXCR6, was modelled using PHYRE and protein - protein docking was performed using ClusPro. The residues which were found to be crucial in interaction with the ligand are THR110, PHE113, TYR114, GLN160, GLN195, CYS251 and SER255. This study can be used as a guide for therapeutic studies of human CXCR6.

Determination of florfenicol residues in swine tissues using high-performance liquid chromatography with ultraviolet photometric detector

  • Chae, Won-Seok;Yoo, Chang-Yeul;Tutkun, Lutfiye;Kim, Suk;Lee, Hu-Jang
    • Journal of Preventive Veterinary Medicine
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    • v.42 no.4
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    • pp.171-176
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    • 2018
  • A study of the tissue depletion of florfenicol (FFC) administered orally to pigs at a dose of 0.05 kg/ton feed for 7 days was performed. Sixteen healthy cross swine were administered with FFC. Four treated animals were arbitrarily selected to be sacrificed 1, 3 and 5 days after the end of treatment. FFC residue concentrations in muscle, liver, kidney, and fat were determined using high-performance liquid chromatography (HPLC) with ultraviolet photometric detector at 230 nm. The correlation coefficient ($R^2$) of the calibration curve for florfenicol amine (FFCa) was > 0.997 and the limits of detection and quantification were 0.012 and $0.040{\mu}g/mL$, respectively. Recovery rates in swine edible tissues ranged from 79.1 to 93.5%. In the FFC-treated group, FFC residues at 3 days post-treatment were below the maximum residue limits (MRLs) in muscle, kidney and fat, and those at 5 days post-administration were below the MRLs in all edible tissues. These results suggest that the withdrawal period of FFC after the drug treatment might be 5 days, which is a sufficient amount of time for reduction of the FFC residues below the MRLs in all edible tissues.

Evaluation of Residual Pesticides in Commercial Agricultural Products Using LC-MS/MS in Korea (LC-MS/MS를 이용한 한국에서 유통되는 농산물의 잔류 농약 평가)

  • Lee, Hwa-Mi;Hu, Soo Jung;Lee, Hyun-Sook;Park, Seung Young;Kim, Nam-Sun;Shin, Yong Woo;Choi, Keun Hwa;Kim, Sung Il;Nam, Seul Yi;Cho, Dae Hyun
    • Korean Journal of Food Science and Technology
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    • v.45 no.4
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    • pp.391-402
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    • 2013
  • Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.