• Title/Summary/Keyword: GC-determination

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Determination of Novel Synthetic 5HT2C Agonist KOPC20010 by Gas-Chromatography/Mass Spectrometry and its Bioavailability in Sprague-Dawley Rats

  • Im, Hye-Yeon;Pae, Ae-Nim;Yang, Ha-Yun;Park, Woo-Kyu;Seo, Ji-Eun;Haque, Md. Mamunul;Kwon, Oh-Seung
    • Journal of Pharmaceutical Investigation
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    • v.41 no.1
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    • pp.31-36
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    • 2011
  • $5HT_{2C}$ receptor among fourteen 5-HT subtypes plays important roles in several disorders such as depression, anxiety, epilepsy, schizophrenia and sleep disorders. The purpose of the study is to investigate pharmacokinetic parameters and bioavailability of a newly synthesized selective agonist of $5-HT_{2C}$ receptor, KOPC-20010 (KP10) in rats after intravenous and oral administration for the development of therapeutic anti-obesity agents. KP10 was administered orally (40 mg/kg) or intravenously (20 mg/kg), blood was collected via a catheter, and analyzed by GC/MSD. The calibration curve of KP10 in plasma and urine showed high linearity ($r^2$ >0.999). The retention times of KP10 in plasma and urine were 8.7 and 9.7 min, respectively. After oral administration of 40 mg/kg, pharmacokinetic parameters were calculated as follows; $C_{max}$ value was $1242.9{\pm}1195.5$ ng/mL at $1.1{\pm}0.6$ hr ($T_{max}$). $AUC_{0->24hr}$ and $AUC_{0>{\infty}}$ were $8034.2{\pm}960.7$ and $10464.1{\pm}681.5\;ng{\cdot}hr/mL$, respectively. The terminal half-life was $21.9{\pm}7.6$ hr. $AUC_{0->24hr}$ and $AUC_{0>{\infty}}$ were $4292.4{\pm}523.0$ and $6111.2{\pm}756.2\;ng{\cdot}hr/mL$, respectively, after 20 mg/kg of intravenous administration. The terminal half-life after intravenous administration was $25.1{\pm}9.4$ hr. Bioavailability of KP10 was determined to 86%. The excretion amount into the urine within 48 hr was approximately 4.7 to 6.7% of the dose administered. These data may be beneficial to the anti-obesity drug development of KP10.

Determination of short-term bioconcentration Factor on BPMC, Carbaryl and Carbofuran in Brachydanio rerio and Xiphophorus hellieri (Brachydanio rerio와 Xiphophorus hellieri를 이용한 BPMC, Carbaryl 및 Carbofuran의 단기간 생물농축계수의 측정)

  • 민경진;전봉식;차춘근;김근배;조영주;송진욱
    • Journal of Food Hygiene and Safety
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    • v.13 no.3
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    • pp.213-220
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    • 1998
  • Bioconcentration factors of some carbamates BPMC, carbaryl and carbofuran were determined. The tested fishes were zebrafish (Brachydanio rerio) and red sword tail (Xiphophorus hellieri). The fishes were exposed to 0.05 ppm, 0.01 ppm, 0.50 ppm, one- hundredth concentration of 96-hrs $LC_{50}$ and one-thousandth concentration of 96-hrs LCso and test periods were 3, 5 and 8 days. Obtained results are summerized as follows: In the case of BPMC and carbaryl, BPMC and carbaryl concentration in zebrafish extract and BCF s of BPMC, carbaryl were lower than those of red sword tail, and increased as increasing test concentration. In the case of same experimental concentrations, BPMC concentration in zebrafish extract and $BCF_s$ of BPMC were decreased as prolonging test periods. In the case of same experimental periods, carbaryl concentration in zebrafish extract and BCF s of carbaryl were decreased as increasing test concentration, especially dropped at 0.50 ppm. Carbofuran did not bioaccumulate in zebrafish for test periods, in the case of red sword tail, it was impossible to calculate on $BCF_s$ data because test concentration of one-hundredth and one-thousandth of 96hrs $LC_{50}$ was under the detecting limit on GC. Test concentration of 0.05 and 0.10 ppm were the same tendency with BPMC and carbaryl. Determined depuration rate conatant were highest on carbofuran, and followed by carbaryl, and BPMC. It is suggested that low BCF of carbofuran is due to its relatively high water solubility and depuration rate, compared to BPMC and carbaryl. Therefore, carbofuran had no little bioconcentration effect on the aquatic ecosystem.

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Identification of the Volatile Compounds in Polyethylene Terephthalate Bottles and Determination of Their Migration Content into Mineral Water (PET 생수병 내 휘발성 물질의 동정 및 이행량 분석)

  • Jung, Eui Min;Kim, Dong Joo;Lee, Keun Taik
    • Korean Journal of Food Science and Technology
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    • v.46 no.1
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    • pp.19-24
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    • 2014
  • This study was carried out to identify the volatile organic compounds (VOCs) in polyethylene terephthalate (PET) bottles and to determine the extent to which VOCs migrate into mineral water during the bottling process and storage. A greater amount of nonanal and decanal was generated from the PET bottles than from the PET preforms. Benzene, ethylbenzene, nonanal, and vinyl benzoate were identified from the PET bottles when the incubation temperature of the headspace solid-phase microextraction (HS-SPME) sampler was set to 60, 80, and $100^{\circ}C$. As the incubation temperature increased, the concentrations of nonanal, vinyl benzoate, and decanal increased significantly. When the high-density polyethylene (HDPE) PET bottle caps were extracted with dichloromethane, the level of Irgafos 168 was found to be $206{\pm}20.1\mu}g/g$. The concentration of 2,4-di-tert-butylphenol in water was $4.80{\pm}0.2{\mu}g/L$. Therefore, it is necessary to avoid exposing PET and HDPE resins to high temperatures during the manufacturing process and storage of bottled water.

Optimization of Synthesis Condition and Determination of Residue for Polyamine Type Flocculant (폴리아민계 고분자 응집제의 합성조건 최적화 및 잔류물분석)

  • Choi, Soo-Young;Park, Lee-Soon;Im, Sung-Hyun;Ryoo, Jae-Jeong;Choi, Sang-June;Hwang, Won-Joo
    • Applied Chemistry for Engineering
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    • v.9 no.7
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    • pp.1043-1046
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    • 1998
  • Aluminium based inorganic flocculants are extensively used in this country in the removal of fine particles present in the raw water for the production of drinking water. These inorganic flocculants, however, have potential hazard of high residual aluminium ions in the treated waters, which is known to be one of the reasons of alzheimer's disease. Inorganic flocculants alone are sometimes incapable of treating water when there are excessive turbidity in the raw water sources due to flooding. A polyamine type polymeric flocculant has long been used to treat raw water in the drinking water production in the European countries and United State of America. The optimum reaction conditions such as mole ratio of epichlorohydrin(EPI) to dimethylamine(DMA), reaction temperature and time for each stage for the pilot scale preparation of polyamine from EPI-DMA was studied in this work. The variation of intrinsic viscosity and flocculating efficiency in the water treatment of the synthesized polyamines were evaluated. The residual materials after polymerization reaction were analyzed by gas chromatography to study the effect of variation of reaction conditions.

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An Application of $^{13}C$ Tracer for the Determination of Primary Productivity and Fatty Acid Production Rate in Shingu Reservoir (신구저수지의 1차 생산 및 지방산 생성속도 결정을 위한 $^{13}C$ 추적자 활용 연구)

  • Lee, Yeon-Jung;Kim, Min-Seob;Shin, Kyung-Hoon;Hwang, Soon-Jin
    • Korean Journal of Ecology and Environment
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    • v.41 no.spc
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    • pp.21-26
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    • 2008
  • The in situ incubation experiment was carried out using $^{13}C$ tracer to determine primary productivity and fatty acid production rate in the shallow, eutrophic Shingu reservoir on 4th July. Particulate organic matter (POM) accounted for 76% in suspended particulate matter (SPM), and average concentration of chlorophyll-${\alpha}$ was $89{\mu}g\;L^{-1}$ in the euphotic layer. Total amount of chlorophyll-${\alpha}$ (Chl-${alpha}$), primary productivity and Chl-${alpha}$ specific productivity in euphotic layer were 112 mg Chl-${alpha}m^{-2}$, 3.53 g C $m^{-2}\;d^{-1}$, 32mg C mg Chl-${\alpha}^{-1}\;d^{-1}$, respectively. The fatty acid composition in newly produced organic matter and suspended organic matter didn't show any significant difference, demonstrating that autochthonous organic matter should be a major source of POM pool. In addition, the fatty acids of bacterial origin were increased through extracellular release of newly photosynthesized DOC, and closely coupled with bacterial assimilation. This result suggests that organic carbon should be actively cycled through the microbial loop in Shingu reservoir in summer.

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.

Changes in 3-Butenyl Isothiocyanate and Total Glucosinolates of Seeds and Young Seedlings during Growth of Korean Chinese Cabbages (배추 종자 및 어린 싹의 성장 시기에 따른 3-butenyl isothiocyanate 및 total glucosinolates 함량 변화)

  • 김연경;김건희
    • Food Science and Preservation
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    • v.10 no.3
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    • pp.365-369
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    • 2003
  • The main objective of this study was to investigate the pattern of glucosinolates, in terms of 3-butenyl isothiocyanate, and total glucosinolates, in different parts of young seedlings and seeds in Korean Chinese cabbages. For determination of glucosinolates, 55 days and Winter pride cultivars of Korean Chinese cabbages seeds and different parts of 1, 3, 5, and 7-day-old seedlings were used for analytical sample preparation provided with an anion exchanges column, and measured by GC and UV-visible Spectrophotometer. The concentration of 3-butenyl ITC was higher in the cotyledon and the hypocotyl parts of 55 days cultivar seedling than those of Winter Pride cultivar. In the cotyledon parts of Winter pride cultivar seedling, 3-butenyl ITC amount was increase to 3-day-old seedling and then reduced. The cotyledon of 55 days cultivar contained the highest concentration of total glucosinolates while those were increased in the hypocotyl and decreased in the root. The level of total glucosinolates was increased to 5-day-old seedling and then decreased in the cotyledon and the hypocotyl parts of seedling in Winter pride cultivar. There was no significant difference of total glucosinolates in the root part. In the seeds, 55 days cultivar concentration was higher than Winter pride cultivar both of 3-butenyl ITC and total glucosinolates. In our study, the levels of 3-butenyl ITC and total glucosinolates depended on cultivars, growth stages, and parts in Korean Chinese cabbage.

EFFECT OF CALCIUM HYDROXIDE REMNANT AS AN INTRACANAL DRESSING ON THE APICAL LEAKAGE (근관내 잔존 Calcium Hydroxide제재가 치근단 미세누출에 미치는 영향)

  • 신수일;조용범
    • Restorative Dentistry and Endodontics
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    • v.26 no.1
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    • pp.77-85
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    • 2001
  • The purpose of this in vitro study was to compare the apical leakage in extracted teeth filled with gutta-percha subsequent to dressing with one of three different calcium hydroxide preparations. Thirty six extracted teeth with single canal were used in this study. After working length determination, canals were prepared with K flexo files to a #40 at the working length. Step-back flaring was produced by using #45, #50 K flexo files and #2, #3, #4 Gates Glidden burs. The teeth were randomly divided into 3 groups of 10 each : the remaining six teeth were used for negative and positive leakage control: Group 1, dressed with pure calcium hydroxide powder (Sigma, USA) mixed with distilled water; Group 2, dressed with Metapaste (Metadent, Korea) ; Group 3, dressed with Vitapex (Neo Dental, Japan). Teeth were sealed with Caviton (GC, Japan) and incubated in 100% humidity, at 37$^{\circ}C$ for 1 wk. All kinds of calcium hydroxide were removed from the canal with a MAF and 5% NaOCl. The canals were filled with AH-26$^{\circledR}$ sealer and gutta-percha using lateral condensation technique, incubated in 100% humidity, at 37$^{\circ}C$ for 2 days for the sealer to be set. The teeth were coated twice with nail varnish except for an area of approximately 2mm surrounding the apical foramen. All specimens were placed in 2% methylene blue solution for 2 days. The root were sectioned longitudinally, the amount of apical leakage was measured to the most coronal part of the root canal to which the dye had penetrated. The independent measurements were made for each root using a stereomicroscope ($\times$40 magnification) and the average was recorded for statistical analysis. The results were as follows ; 1. The mean of apical leakage in group of pure calcium hydroxide ranged 0.102$\pm$0.156mm, in Metapaste$^{\circledR}$ ranged 0.062$\pm$0.069mm, and in Vitapex$^{\circledR}$ ranged 0.067$\pm$0.072mm. 2. Group of pure calcium hydroxide exhibited more leakage than those of 2 manufactured calcium hydroxide preparations, but it was not statistically significant. 3. Group of water-based Metapaste$^{\circledR}$ showed lesser leakage than that of oil-based Vitapex$^{\circledR}$, but it was not statistically significant.

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A Correlation Study between the Environmental, Personal Exposures and Biomarkers for Volatile Organic Compounds (대기 중 휘발성유기오염물질의 환경, 개인 및 인체 노출의 상관성 연구)

  • Jo, Seong-Joon;Shin, Dong-Chun;Chung, Yong;Breysse, Patrick N.
    • Environmental Analysis Health and Toxicology
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    • v.17 no.3
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    • pp.197-205
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    • 2002
  • Volatile organic compounds (VOCs) are an important public health problem throughout the world. Many important questions remain to be addressed in assessing exposure to these compounds. Because they are ubiquitous and highly volatile, special techniques must be applied in the analytical determination of VOCs. Personal exposure measurements are needed to evaluate the relationship between microenvironmental concentrations and actual exposures. It is also important to investigate exposure frequency, duration, and intensity, as well as personal exposure characteristics. In addition to air monitoring, biological monitoring may contribute significantly to risk assessment by allowing estimation of absorbed doses, rather than just the external exposure concentrations, which are evaluated by environmental and personal monitoring. This study was conducted to establish the analytic procedure of VOCs in air, blood, urine and exhaled breath and to evaluate the relationships among these environmental media. The subjects of this study were selected because they are occupationally exposed to high levels of VOCs. Environmental, personal, blood, urine and exhalation samples were collected. Purge & trap, thermal desorber, gas chromatography and mass selective detector were used to analyze the collected samples. Analytical procedures were validated with the“break through test”, 'quot;recovery test for storage and transportation”,“method detection limit test”and“inter-laboratory QA/QC study”. Assessment of halogenated compounds indicted that they were significantly correlated to each other (p value < 0.01). In a similar manner, aromatic compounds were also correlated, except in urine sample. Linear regression was used to evaluate the relationships between personal exposures and environmental concentrations. These relationships for aromatic and halogenated are as follows: Halogen $s_{personal}$ = 3.875+0.068Halogen $s_{environmet}$, ($R^2$= .930) Aromatic $s_{personal}$ = 34217.757-31.266Aromatic $s_{environmet}$, ($R^2$= .821) Multiple regression was used to evaluate the relationship between exposures and various exposure deter-minants including, gender, duration of employment, and smoking history. The results of the regression model-ins for halogens in blood and aromatics in urine are as follows: Halogen $s_{blood}$ = 8.181+0.246Halogen $s_{personal}$+3.975Gender ($R^2$= .925), Aromatic $s_{urine}$ = 249.565+0.135Aromatic $s_{personal}$ -5.651 D.S ($R^2$ = .735), In conclusion, we have established analytic procedures for VOC measurement in biological and environmental samples and have presented data demonstrating relationships between VOCs levels in biological media and environmental samples. Abbreviation GC/MS, Gas Chromatography/Mass Spectrometer; VOCs, Volatile Organic Compounds; OVM, Organic Vapor Monitor; TO, Toxic Organicsapor Monitor; TO, Toxic Organics.

Sample Preparation for Quantitative Determination of Bisphenols in Canned Beverages Coated with Epoxy by RP-HPLC (RP-HPLC 에 의한 에폭시 통조림관 음료 중 비스페놀류의 분석을 위한 시료의 전처리)

  • Kang, Kyung-Mo;Lim, Heung-Youl;Shin, Hyo-Sun
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.1029-1034
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    • 2000
  • A suitable method of sample treatments to minimize the analytical interferences was presented in order to determine bisphenols [bisphenol F (BPF), bisphenol A (BPA), bisphenol F diglycidyl ether (BFDGE), and bisphenol A diglycidyl ether (BADGE)] in various canned beverages coated with epoxy resin by the reversephase high performance liquid chromatography (RP-HPLC) equipped with a fluorescence detector and the gas chromatography with mass selective detection. The recovery test of bisphenols was performed using 1, 5, and 10 ${\mu}g/L$ bisphenols spiked beverages with the combined technique of the solid-phase extraction (SPE) and the liquid-phase extraction (LPE). Both BPA and BADGE showed quite adequate resolutions in HPLC-chromatograms. The recoveries of BPA obtained by LPE with diethyl ether were higher than those obtaind with methylene chloride on coffee, shikhye and fruit juice. For cola and tea, the recoveries of BPA obtaind by SPE were higher than those by LPE with diethyl ether. The recoveries of BADGE were less than those of BPA for all beverage samples treated by either SPE or LPE method. In survey of bisphenols for eighteen commercial canned beverage samples, BPA contents of coffee, cola, tea, shikhye, and fruit juice were in the range of $1.3{\sim}11.6,\;0.5{\sim}0.9,\;1.0{\sim}1.3,\;2.4{\sim}7.9$, and $3.0{\sim}3.4\;{\mu}g/L$, respectively, but there was no detection of BPA in beer sample.

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