• Title/Summary/Keyword: gas chromatography-nitrogen phosphorus detector

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Development of Simultaneous Analysis for the Multi-residual Pesticides in the Ginseng Extract using Gas Chromatography (인삼농축액에서 GC를 이용한 잔류농약 동시다성분 분석법의 개발)

  • Shin Yeong-Min;Lee Seon-Hwa;Son Yeong-Uk;Jeong Ji-Yoon;Jeoung Seoung-Wook;Park Heung-Jai;Kim Sung-Hun;Won Young-Jun;Lee Chang-Hee;Kim Woo-Seong;Hong Moo-Ki;Chae Kab-Ryong
    • Journal of Environmental Science International
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    • v.15 no.1
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    • pp.85-94
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    • 2006
  • The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

Pharmacokinetics of Propentofylline and the Quantitation of Its Metaolite Hydroxypropentofylline in Human Volunteers

  • Kwon, Oh-Seung;Chung, Youn-Bok;Kim, Min-Hee;Hahn, Hoh-Gyu;Rhee, Hee-Kyung;Ryu, Jae-Chun
    • Archives of Pharmacal Research
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    • v.21 no.6
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    • pp.698-702
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    • 1998
  • Propentofylline (PPF, 3-methyl-1-(5-oxohexyl)-7-propylxanthine) has been reported to be effective for the treatment of both vascular dementia and dementia of the Alzheimer type. The pharmacological effects of PPF may be exerted via the stimulation of nerve growth factor, increased cerebral blood flow, and inhibition of adenosine uptake. The objectives of this experiment are to determine the kinetic behavior of PPF, to identify, and to quantify its metabolite in human. Blood samples were obtained from human volunteers following oral administration of 200mg of PPF tablets. For the identification and quantification of the metabolite, 3-methyl-1-(5-hydroxyhexyl)-7-propylxanthine (PPFOH), PPFOH was synthesized and identified by gas chromatography/mass spectroscopy (GC/MS) and $^1H$-nuclear magnetic resonance spectroscopy. The molecular weight of synthesized metabolite is 308 dalton. The PPF and PPFOH in plasma were extracted with diethyl ether and identified by electron impact GC/MS. The plasma concentrations of PPF and PPFOH were determined by gas chromatography/nitrogen phosphorus detector in plasma and their pharmacokinetic parameters were determined. The mean half-life of PPF was 0.74 hr. The areas under the curve (AUCs) of PPF and PPFOH were 508 and 460ng.hr/ml, respectively. $C_{max}$ of PPF was about 828.4ng/ml and the peak concentration was achieved at about 2.2 hr ($T_{max}$). These results indicate that PPF is rapidly disappeared from blood due to extensive metabolism into PPFOH.

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Bioequivalence Assesment of Tiropramide in Korean Male Volunteers

  • Park, Young-Jin;Chung, Youn-Bok;Kwon, Oh-Seung
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 2002.07a
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    • pp.205-205
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    • 2002
  • Two formulations of tiropramide {(${\pm}$)${\alpha}$-(benzoylamino)-4-[2-(diethylamino)-ethoxy]-N,N-dipropyl-benzenepropanamide hydrochloride}, an antispasmodic agent, were orally administered to 16 healthy Korean male volunteers by Latin crossover design with the purpose of evaluating bioeqivalence and phamacokinetics of tiropramide. Tiropramide in human plasma was determined by a gas chromatography/nitrogen phosphorus detector. Detection limit of tiropramide was 5 ng/ml. C$\_$max/ values in test and reference formulations were 93.9 ${\pm}$ 54.3 and 96.4 ${\pm}$ 51.6 ng/ml, respectively. AUC$\_$0\longrightarrowlast/ and AUC$\_$0\longrightarrowinf/ were, respectively, 330.7 ${\pm}$ 193.9 and 349.5 ${\pm}$ 205.3 ng.hr/ml for test formulation, 348.9 ${\pm}$ 207.7 and 380.8 ${\pm}$ 239.0 ng.hr/ml for reference formulation. Terminal half-life was 2.3-2.6 hr. Bioavailability differences for C/aub max/ and AUC$\_$0\longrightarrowlast/ were 2.48% and 5.22%, respectively. Minimum detection differences were less than 20% in both C$\_$max/ AUC. Based on this results, two formulations of tiropramide were considered to be bioequivalent

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Simultaneous Determination of Simetryn and Buprofezin by Gas Chromatography with Nitrogen Fhosphorus Detector (GC-NPD를 이용한 Simetryn과 Buprofezin의 동시 분석법 연구)

  • Kim Eunjeung;Kim Sungdan;Lee Jaekyoo;Kim Soojin;Lee Sangmi;Han Sunhee;Kang Heegon
    • Journal of Food Hygiene and Safety
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    • v.20 no.3
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    • pp.159-164
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    • 2005
  • This method was described for the simultaneous determination of simetryn and buprofezin in rice, vegetables, and fruits by gas chromatography(GC) with nitrogen phosphorus detector. The GC method of simetryn and buprofezin was shown to give a linear detection ranges between $0.019\sim9.306mg/kg,\;0.023\sim11.27mg/kg$, respectively. For evaluation of GC method, simetryn spiked into rice, vegetables and fruits at the level of 4.653mg/kg was determined. The recoveries of simetryn by GC method were ranged from 57.9 to $115.9\%$. For evaluation of GC method, buprofezin spiked into rice, vegetables and fruits at the level of 2.817mg/kg was determined. The recoveries of buprofezin by GC method were ranged from 56.5 to $121.5\%.$

Monitoring of Pesticide Residues and Risk Assessment for Medicinal Plants (국내 유통 약용식물 중 잔류농약 모니터링 및 위해성 평가)

  • Ahn, Ji-Woon;Jeon, Young-Hwan;Hwang, Jeong-In;Kim, Jeong-Min;Seok, Da-Rong;Lee, Eun-Hyang;Lee, Sung-Eun;Chung, Duck-Hwa;Kim, Jang-Eok
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.13-18
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    • 2013
  • This study was conducted to monitor residual pesticides in ginseng and balloon flower roots and to assess their risk to human health. All of 112 samples consisted of ginseng and balloon roots were purchased from traditional domestic markets and supermarkets in nine provinces of Korea in 2012. Multi-residue analysis of 122 pesticides was conducted and the analysis was performed by gas chromatography-electron capture detector, gas chromatography- nitrogen/phosphorus detector, and high-performance liquid chromatography. Seven pesticides were detected in 12 root samples and the detection rate was 10.7%. The detected twelve root samples were 10 ginseng root samples and 2 balloon root samples. Pesticides detected in root samples were procymidone, kresoxim-methyl, endosulfan, cypermethrin, tralomethrin, tetraconazole and chlorfluazuron. Among them, two pesticides as tetraconazole in a balloon flower root and cypermethrin in a ginseng root exceeded the recommended maximum residue limit set by Korea Food and Drug Administration. Five pesticides detected from 10 root samples were identified as unregistered pesticides in Korea. In order to do risk assessment with Korean medicinal plant consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to %ADI values. The range of %ADI values was from 0.006% to 0.333%. Taken together, it demonstrates the pesticides found in the two root samples were below the safety margin, indicating no effect on human health.

Monitoring of Pesticide Residues and Risk Assessment for Fruits in Market (국내 유통 과실류의 잔류농약 모니터링 및 위해성 평가)

  • Ahn, Ji-Woon;Jeon, Young-Hwan;Hwang, Jeong-In;Kim, Jeong-Min;Seok, Da-Rong;Lee, Eun-Hyang;Lee, Seong-Eun;Chung, Duck-Hwa;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.32 no.2
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    • pp.142-147
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    • 2013
  • BACKGROUND: This study was conducted to monitor residual pesticides in domestic agricultural products and to assess their risk to human health. METHODS AND RESULTS: 123 samples containing both general and environment-friendly certified agricultural products were purchased from traditional domestic markets and supermarkets in six provinces of Korea. Multiresidue analyses of one hundred twenty-two pesticides except for herbicides were performed with gas chromatography-electron capture detector, gas chromatography-nitrogen/phosphorus detector, and high-performance liquid chromatography. Sixteen pesticides were detected in 45 agricultural product samples, which were 38 general, 6 low pesticide and 1 of GAP agricultural product samples and the detection rate was 33.6%. Pesticides detected in agricultural product samples were cypermethrin, lufenuron, fenvalerate, bifenthrin, chlorfenapyr and iprodione. Residual concentration of 18 samples were exceeded the recommended maximum residue limit set by Ministry of Food and Drug Safety and two kinds of unregistered pesticides in korea were also detected in two samples. CONCLUSION(S): In order to do risk assessment by agricultural products consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to %ADI values. The range of %ADI values was from 0.038% to 2.748%. Taken together, it demonstrates the pesticides found in agricultural products samples were below the safety margin, indicating no effect on human health.

Monitoring of Pesticide Residues and Risk Assessment in Some Fruits on the Market in Incheon, Korea (인천지역 유통 과일 중 잔류농약 모니터링 및 위해성 평가)

  • Chung, Se Jin;Kim, Hye Young;Kim, Ji Hyeung;Yeom, Mi Suk;Cho, Joong Hee;Lee, Soo Yeon
    • Korean Journal of Environmental Agriculture
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    • v.33 no.2
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    • pp.111-120
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    • 2014
  • BACKGROUND: This study was conducted to investigate the levels of pesticide residues in fruits and to assess their risk to human health. METHODS AND RESULTS: Monitoring of 215 samples of fruits collected from local markets in incheon during 2013 was performed. 259 pesticides were analyzed by multi-residue method and Quick, Easy, Cheap, Effective, Rugged, and safe/Mass/Mass(QuEChERS/MS/MS) method using Gas Chromatography-Electron Capture Detector/Nitrogen Phosphorus Detector(GC-ECD/NPD), GC-MS, LC(Liquid Chromatography-Mass/Mass(LC-MS/MS) and High Performance Liquid Chromatography-Photodiode Array/Fluorescence Detector(HPLC-PDA/FLD). In 56.3% of the samples detected pesticide residues and were not found to exceed Maximum Residue Limits(MRL). The highest detected samples were found in citrus fruits(83.9%). Among the detected compounds, carbendazim(13.1%), imazalil (11.7%), thiabendazole(10.7%) and fludioxonil(9.8%) were frequently found in fruits. A risk assessment of pesticide residues in fruits was performed by calculating Estimated Daily Intake(EDI) and Acceptable Daily Intake(ADI). Also, we were evaluated removal efficiency of pesticide residues by washing and peeling. The removal efficiency of pesticide residues in citrus and tropical fruits by peeling processes were 91.6%. After the washing process, the removal rates were 43.1%(Cherry, Grape, Blueberry). CONCLUSION: The level of pesticide residues in fruits was within the MRL. The range of %ADI values was from 0.00011 to 0.98795%. The process of washing or peeling reduces the level of pesticide residues. The results of this research concluded that the detected pesticides are not harmful to human being.

A survey on pesticide residues of imported fruits circulated in Gyeonggido (경기도내 유통 수입과실류의 잔류농약 실태조사)

  • Cho, Yun-Sik;Kang, Jeong-Bok;Kim, Yang-Hee;Jeong, Jin-A;Huh, Jeong-Weon;Lee, So-Hyun;Lim, Young-Sik;Bae, Ho-Jeong;Kang, Heung-Gyu;Lee, Jeong-Hee;Jung, Eun-Sook;Lee, Byoung-Hoon;Park, Yong-Bok;Lee, Jong-Bok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.195-201
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    • 2012
  • We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

Simultaneous Determination of Pesticide Residues in Soils by Dichloromethane Partition - Adsorption Chromatography - GC-ECD/NPD Analytical Methods (Dichloromethane 분배 - 흡착 크로마토그래피 - GC-ECD/NPD 분석법에 의한 토양잔류농약 다성분 분석)

  • Kim, Chan-Sub;Lee, Byung-Moo;Park, Kyung-Hun;Park, Byung-Jun;Park, Jae-Eup;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.361-370
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    • 2010
  • Considering the efficiencies of the preparation process at each stage obtained in previous studies, the analytical determination method was established for multi-pesticide residues in soils. It consist of the acetone-extraction, the dichloromethane-partition, the Florisil or silica-gel chromatography and the gas chromatography analysis equipped with the electron capture detector and the nitrogen-phosphorus detector. In the soil recovery test by Florisil clean-up system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 165 pesticides for paddy soil, 169 pesticides for upland soil and 159 pesticides in both soils through the tested 183 pesticides. And in the soil recovery test by silica-gel system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 154 pesticides for paddy soil, 145 pesticides for upland soil, and 134 pesticides in both soils.

Distribution of Organophosphorus Pesticides in some Estuarine Environments in Korea

  • Yu Jun;Lee Dong Ho;Kim Kyung Tae;Yang Dong Beom;Yang Jae Sam
    • Fisheries and Aquatic Sciences
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    • v.4 no.4
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    • pp.201-207
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    • 2001
  • To study the distribution of organophosphorus pesticides which are extensively used for agriculture in Korea. Sea water samples were taken from 4 coastal areas during May and August of 1997 and sediment samples were collected from two coastal areas in August of 1997. These samples were analyzed using a Gas Chromatography/Nitrogen Phosphorus Detector (GC/NPD). In August the most commonly found organophosphorus pesticides in the surface waters of Kunsan area were IBP < S-Benzyl O,O-di-isopropyl phosphorothioate > $(m=432.5ng\;L^{-1})$ and EDDP < O-ethyl S,S-diphenyl phosphorodithioate > $(m=37.4ng\;L^{-1}) $ which are largely used between June and September to prevent rice blast disease. In Danghang Bay, dry fields located near the mouth of the estuary seemed to affect the concentrations of certain organophosphorus pesticides in the surface waters. Since organophosphorus pesticides applied in the watershed are rapidly decomposed while being transported along freshwater streams, watershed size is not proportional to the concentrations of these pesticides in the coastal waters. Pesticides concentrations measured in August were compared with those in May. IBP concentrations in coastal waters were about an order of magnitude higher in August than in May. Temporal and geographical distribution of individual organophosphorus pesticides is likely to be affected by types of agricultural practices in the watershed. Chloropyrifos was the most important of the organophosphorus pesticides in the sediments of the study area because of its persistent nature and high affinity to particulates.

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