• Title/Summary/Keyword: Triethylamine

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Synthesis and Characterization of Waterborne Polyurethane Using Nanoclay (나노 클레이를 사용한 수분산 폴리우레탄의 합성과 특성)

  • Cheon, Jung Mi;Jeong, Boo Young;Yoo, Chong Sun;Park, Duck Jei;Bae, Jae Kyu;Chun, Jae Hwan
    • Journal of Adhesion and Interface
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    • v.8 no.4
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    • pp.1-7
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    • 2007
  • Waterborne polyurethane (WPU) which is environment friendly has been rapidly used in coating and adhesive industries. However, the WPU is deficient in chemical resistance, thermal resistance, and mechanical property compared to solvent-based polyurethane. In this study, the WPU was synthesized from two types of polyester polyols, 4,4-dicyclohexylmethane diisocyanate ($H_{12}MDI$), dimethylolpropionic acid (DMPA), triethylamine (TEA) and ethylenediamine (EDA), organophilic nanoclay. The thermal stability, mechanical property of the WPU nanocomposite dispersion increased with increasing clay concentration. Especially, their peel strength showed their maximum value at 3 wt% of organophilic nanoclay contents.

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Study on the Synthesis of N,N'-Dicyclohexylcarbodiimide from N,N'-Dicyclohexylurea (디사이클로헥실우레아로부터 디사이클로헥실카르보디이미드의 합성에 관한 연구)

  • Kim, Jae Young;Chung, Dae-Won
    • Applied Chemistry for Engineering
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    • v.22 no.3
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    • pp.319-322
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    • 2011
  • N,N'-Dicyclohexylcarbodiimide (DCC) known as powerful dehydrating reagent in amide or ester synthesis is converted into N,N'-dicyclohexylurea (DCU) during the reaction. In the paper, DCU was recovered from the reaction for the synthesis of the hydrophilic derivative of ${\beta}$-sitosterol, and the purification of the recovered DCU and the dehydration of DCU into DCC were investigated. In the presence of tosyl chloride, (TsCl) and triethylamine (TEA), DCU was converted into DCC, and the optimum molar ratio of [DCU] : [TsCl] : [TEA] was found to be 1.0 : 1.5 : 3.0. Pure DCC was obtained with a 46% yield by the sublimation after the purification process, and characterized by GC/MS, FT-IR and $^{13}C-NMR$.

Determination and Survey of Fluoroquinolones Residue in Chicken Muscle by HPLC with Fluorescence Detector (액체크로마토그래피-형광검출기를 이용한 닭고기 중 플루오로퀴놀론계 항균물질 정량분석 및 잔류조사)

  • 박은정;임지흔;이성모
    • Journal of Food Hygiene and Safety
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    • v.19 no.1
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    • pp.12-18
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    • 2004
  • Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

Adsorption Characteristics on Organic Solvents Diluted in Supercritical Carbondioxide Measured by Chromatography and IR Spectroscopy (적외분광법과 크로마토 측정기법을 이용한 초임계 이산화탄소 중에 희석시킨 유기용매의 흡착특성)

  • Jin, Do-Won;Kim, Young-Il;Park, Dong-Won
    • Applied Chemistry for Engineering
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    • v.9 no.1
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    • pp.76-81
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    • 1998
  • Physical adsorption on a silica gel(pore size of 80 nm, particle size of $10{\mu}m$)has been studied for binary mixture of acetone diluted in $CO_2$ by use of a FTIR transmission technique and we have compared the result of FTIR transmission technique with that of a chromatographic technique. Measurements were made at 313.2 K and under pressures up to 15MPa. As the pressure increases from 0.1MPa, the IA(Integral Absorbance) of the hydrogen-bonded OH groups interacting with acetone and adsorbed amount by use of a chromatographic technique increases at first, and reaches a maximum at a pressure below the critical pressure of $CO_2$, and then the intensities decrease gradually with increasing pressure. It is found that the pressure dependency of the chromatographic isotherm is a little larger than that of spectroscopic isotherm in the supercritical fluid region. This difference might be attributable to the weaker van der Waals force and relatively stronger hydrogen-bonding force influencing the adsorption of acetone on the sllica gel. The unique spectroscopic characteristics of amine group which vibrational frequencies of hydroxyl groups on the silica gel surface shift downward to about $1300cm^{-1}$ were measured from experimental result of triethylamine diluted in $CO_2$ or $N_2$.

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Rapid Gas Chromatographic Screening of Dairy Products for Volatile and Nonvolatile Organic Acids (기체크로마토그래피법에 의한 유제품내 휘발성 및 비휘발성 유기산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook;Choi, Kyoung-Sook
    • Korean Journal of Food Science and Technology
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    • v.26 no.6
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    • pp.665-669
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    • 1994
  • A rapid gas chromatographic (GC) profiling method was applied to dairy products (milk and cheeses) for the simultaneous analysis of volatile and nonvolatile organic acids. Cheese samples were first made into aqueous samples by dissolving in water. The aqueous samples were then extracted with organic solvents after the acidification and NaCI saturation. The organic layers (diethyl ether : hexane= 1 : 1) were extracted with $NaHCO_3$ saturated solution with subsequent solid-phase extraction of the aqueous phases using Chromosorb P column/diethyl ether followed by triethylamine treatment. The resulting triethylammonium salts of acids were directly converted into volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC, and GC-mass spectrometry. From milk and four cheese samples studied, 31 organic acids including 21 fatty acids and other hydroxy and dioic acids were tentatively identified. The amounts of the fatty acids were different among the kinds of cheese and thus the simplified retention index (RI) spectra of organic acids were useful for the visual pattern recognition of each sample, when the Direct Comparision method between cheese and a blind sample were attempted, it was quickly recognized to be a gouda cheese with the 999 ppt match quality value.

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Synthesis of Trifluoromethylated Dihydro-1,4-oxathiin Carboxanilides and Their Fungicidal Activity (삼불화메틸기가 포함된 디히드로-1,4-옥사티인 카르복스아닐리드 유도체의 합성과 살균 활성)

  • Nam, Kee-Dal;Kim, Jin-Cheol;Cho, Kwang-Yun;Hahn, Hoh-Gyu
    • Applied Biological Chemistry
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    • v.44 no.3
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    • pp.191-196
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    • 2001
  • ${\alpha},{\beta}$-Unsaturated carboxanilides 5 with trifluromethylated dihydro-1,4-oxathiins were synthesized for the development of new agrochemical fungicide. Chlorination of trifluoromethylated ${\beta}-keto$ ester 6 followed by the reaction with 1,2-mercaptoethanol gave intermediate 1,4-oxathiane 11. Without purification of 11, substitution of hydroxy group by chlorine, followed by dehydrochlorination of 10 in the presence of triethylamine afforded trifluoromethylated dihydro-1,4-oxathiin ethyl ester 9. Acylation of the hydroxy group of the carboxylic acid 12 followed by treatment of various amines gave the corresponding trifluoromethylated dihydro-1,4-oxathiin carboxamides 5. Antifungal screening (in vivo) of the synthesized compounds against typical plant diseases, which include rice blast, rice sheath blight, cucumber gray mold, tomato late blight, wheat leaf rust, and barley powdery mildew, was carried out. Where meta position of the phenyl group was substituted with isopropoxy or isopropyl group, excellent antifungal activities against rice sheath blight and wheat leaf rust were detected.

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Determination of Terazocin in Human Plasma by Liquid Chromatography and Bioequivalence Study of Teratonin® Tablets (액체크로마토그래프법에 의한 사람 혈장 중 테라조신의 정량 및 테라토닌® 정의 생물학적 동등성)

  • Cho, Eun-Sook;Kang, Sung-Ha;Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.32 no.2
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    • pp.119-125
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    • 2002
  • A rapid, selective and reproducible high-performance liquid chromatographic method has been developed for the determination of terazocin in human plasma. Terazocin plus the internal standard, prazocin hydrochloride, were extracted from alkalified plasma with tert-butylmethyl ether, back-extracted into 0.05% phosphoric acid. Fifty ${\mu}l-portions$ of extract were injected onto a octadecylsilane column and eluted with a mixture of acetonitrile, water and triethylamine (30 : 70 : 0.1 v/v, adjusted to pH 5.0 with dilute phosphoric acid) at a flow rate of 1.0 ml/min. The fluorescence intensity of column eluents was monitored at excitation wavelength of 250 nm and emission wavelength of 370 nm. No interference peaks were observed. The practical limit of quantitation was 5 ng/ml for terazocin. The average intraday and interday coefficients of variation were 4.15 and 3.54%, respectively. Also intraday and interday precisions over the range $5{\sim}60\;ng/ml$ were $0.49{\sim}2.92\;and\;0.38{\sim}5.12%$, respectively. The bioequivalence of two terazosin tablets, the $Hytrine^{\circledR}$ (Il Yang Pharmaceutical Co., Ltd.) and the $Teratonin^{\circledR}$ (Sam-A Pharmaceutical Co., Ltd.), was evaluated according to the guideline of Korea Food and Drug Administration (KFDA). Sixteen healthy male volunteers $(24.6{\pm}2.0\;years\;old)$ were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After one tablet containing 2 mg of terazosin was orally administered, blood was taken at predetermined time intervals and the concentration of terazosin in plasma was determined with a HPLC method using spectrofluorometric detector. AUC was calculated by the linear trapezoidal method. $C_{max}\;and\;T_{max}$ were compiled from the plasma drug concentration-time data. Analysis of variance (ANOVA) was utilized for the statistical analysis of the parameters. The results showed that the differences in $AUC_t,\;C_{max}\;and\;T_{max}$ between the two preparations were 0.21 %, 5.53% and 8.82%, respectively. The powers $(1-{\beta})\;for\;AUC_t,\;C_{max}\;and\;T_{max}$ were >99%, 97.49%, and 33.26%, respectively. Minimum detectable differences $({\Delta},\;%)\;at\;{\alpha}=0.1\;and\;1-{\beta}=0.8$ and the 90% confidence intervals were all less than ${\pm}20%$ except for $T_{max}.\;AUC_t\;and\;C_{max}$ met the criteria of KDFA for bioequivalence, indicating that $Teratonin^{circledR}$ tablets are bioequivalent to $Hytrine^{circledR}$ tablets.

A study on the residues of fluoroquinolones in hen's eggs consumed in Incheon Metropolitan city (인천광역시에서 유통되는 계란의 플루오로퀴놀론계 항균물질 잔류 실태 조사)

  • Park, Eun-Jeong;Lim, Ji-Huen;Lee, Sung-Mo;Im, Jeong-Soo;Oh, Dae-Kyu
    • Korean Journal of Veterinary Service
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    • v.31 no.3
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    • pp.385-395
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    • 2008
  • This study was carried out to investigate the residue level of fluoroquinolones in hen's general eggs and specific eggs by microbiological assay method and high performance liquid chromatography (HPLC) method. HPLC separation was carried out by reversed phase chromatography on a Symmetry $C_{18}$ (250${\times}$4.6 mm, $5{\mu}m$ particle size) with a phase composed of distilled water (containing 0.4% triethylamine and phosphoric acid) : Methanol (780 : 220, v/v), pumped isocratically at a flow rate of 1.0ml/min. A fluorescence detector was utilized with an excitation wavelength of 278nm and an emission wavelength of 456nm. The calibration curves were linear $({\gamma}^2{\geq}0.999)$ over a concentration range of $0.025{\sim}0.4{\mu}g/ml$. Average recoveries of the five fluoroquinolones in whole eggs at fortified levels of $0.05{\sim}0.2{\mu}g/g$ were ranged mean $78.1{\sim}91.7%$ and low coefficient of variation was less than 10% for all analysed samples. The limits of detection and limits of quantification for whole eggs were $1.2{\sim}6.0ng/g$ and $2.3{\sim}9.1ng/g$, respectively. Only one hen's general eggfrom chicken farm in Incheon was detected with the residual fluoroquinolones (Microbiological assay method; 1 of 47 general eggs) ; the range of residual concentration enrofloxacin was 0.12ppm. Those in food stores were detected with the residual fluoroquinolones (Microbiological assay method; 4 of 88 general eggs) ; the ranges of residual concentration enrofloxacin were $0.15{\sim}2.2 ppm$, ciprofloxacin $0.01{\sim}0.06ppm$, and hen's specific eggs (40) in food stores were not detected. For the microbiological assay method of fluoroquinolones in hen's eggs, as the results of comparative analysis, the disc diffusion method with E coli may be a little highly detected for the residual fluoroquinolones.

Rapid Gas Chromatographic Screening of Vegetable Oils for Free Fatty Acids (기체크로마토그래피법에 의한 식물성 유지내 유리 지방산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.373-378
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    • 1993
  • A rapid gas chromatographic profiling method for the simultaneous analysis of free fatty and other acids was applied to vegetable oils. Oil samples were dissolved in dichloromethane and the free acids were extracted with saturated $NaHCO_3$ solution. The aqueous extract was acidified and then loaded onto the Chromosorb P column for the extraction. The acids were eluted with diethyl ether selectively from Chromosorb P column and were treated with triethylamine to prevent the losses of volatile acids. Several long chain fatty acids were detected from soybean oil, rice-bran oil, sesame oil and perilla oil. Various organic acids including odd number fatty acids were detected in crude oil, especially sesame oil. Arachidic acid from perilla oil and vanillic acid from sesame oil, which were not reported before were detected. The content ratio of free linoleic acid to oleic acid was $1.02{\sim}1.18$, which was similar to the reported data. When the GC profile of organic acids were simplified to their corresponding retention index spectra of bar graphical forms, they presented characteristic pattern of each vegetable oil that can be quickly recognized.

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A Study on the Effect of Different Functional Groups in Anion Exchange Membranes for Vanadium Redox Flow Batteries (바나듐 산화환원 흐름전지를 위한 음이온교환막의 관능기에 따른 특성 연구)

  • Lee, Jae-Myeong;Lee, Mi-Soon;Nahm, Ki-Seok;Jeon, Jae-Deok;Yoon, Young-Gi;Choi, Young-Woo
    • Membrane Journal
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    • v.27 no.5
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    • pp.415-424
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    • 2017
  • Commonly cation exchange membranes have been used for vanadium redox flow batteries. However, a severe vanadium ion cross-over causes low energy efficiency. Thus in this study, we prepared 3 different anion exchange membranes to investigate the effect on the membrane properties such as vanadium ion cross-over and long term stability. The base membranes were prepared by an electrolyte pore filling technique using vinyl benzyl chloride (VBC), divinylbenzene (DVB) within a porous polyethylene (PE) substrate. Then 3 different functional amines were introduced into the base membranes, respectively. These resulting membranes were evaluated by physico-chemical properties such as ion exchange capacity, dimensional stability, vanadium ion cross-over and membrane area resistance. Conclusively, TEA-functionalized membrane showed longest term stability than other membranes although all the membranes are similar to coulombic efficiency.