• Title/Summary/Keyword: amine

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Ruthenium Complex Catalyzed Reaction of Diols or Triol with Amines (루테늄 착물 촉매를 이용한 디올 및 트리올과 아민과의 반응)

  • Sang Chul Shim;Young Zoo Youn;Jae Wook Lee;Dong Yeob Lee;Jae Goo Shim;Ju Hee Kim;Keun Tae Huh
    • Journal of the Korean Chemical Society
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    • v.37 no.11
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    • pp.967-973
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    • 1993
  • ${\alpha},{\omega}$-Diols such as 1,6-hexanediol and 1,7-heptanediol react with secondary amines in the presence of catalytic amount of ruthenium complex at 180$^{\circ}$C for 24 hrs to give the corresponding diamino compounds in good yields. The yield of diamino compound was affected by the molar ratio of ${\alpha},{\omega}$-diol to secondary amine. The reaction was also affected by the nature of the phosphorus ligands employed. On the other hand, aromatic primary amines react with 1,2,6-hexanetriol in the presence of RuCl_3{\cdot}H_2O-3PPh_3$ at 180$^{\circ}$C for 3 hours under argon atmosphere to give selectively 1-substituted aryl-3-hydroxyperhydroazepines in good yields. Selective synthesis of these products show that two primary hydroxy groups (1,6-positions) oxidize predominantly than secondary hydroxy group (2-position) by ruthenium-phosphorus complex. The yields were decreased according to the order of para-, meta- and ortho-substituent.

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Analysis Method of N-Nitrosamines in Human Urine by LC-MS/MS System (LC-MS/MS 시스템을 이용한 소변 중 N-니트로사민류 분석법 확립)

  • Park, Na-Youn;Jung, Woong;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.61 no.2
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    • pp.51-56
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    • 2017
  • N-nitrosamines are the nitroso compounds which are produced by nitrosation reactions of the secondary amine and nitrite under acidic conditions. Approximately 300 species of N-nitrosamine have been tested for carcinogenicity in laboratory experiments, with 90% of them demonstrated carcinogenic effects different animal species, including higher primates. In 1978, IARC classified NDMA and NDEA as Group 2A, and NDPA, NDBA, NPIP, NPYR and NMOR as Group 2B. In this study, we established pretreatment and analytical method for N-nitrosamines (NDMA, NDEA, NMEA, NDPA, NDBA, NPIP, NPYR and NMOR) in human urine for biological monitoring of N-nitrosamines. The analytes were extracted using solid phase extraction (SPE), then quantitative analysis was performed by LC-(APCI)-MS/MS. The accuracies of the established method were between 85.8~108.7% and precisions were lower than 20%. The limit of detection (LOD) were between 0.0002 (NDBA) and 0.0793 (NDMA) ng/ml. The linearity obtained was satisfying for the 8 N-nitrosamines, with a coefficient of determination ($r^2$) higher than 0.999. The mean concentrations of N-nitrosamines in the urine were 2.645 mg/g creatinine for NDMA, 0.067 mg/g creatinine for NDEA, 0.009 mg/g creatinine for NMEA, 0.011 mg/g creatinine for NDBA, 0.271 mg/g creatinine for NPIP and 0.413 mg/g creatinine for NPYR. NDPA and NMOR were not detected. It can be used as a instrumental methodology for evaluation and risk assessment of human exposure to N-nitrosamines for the further research.

Synthesis and Characterization of Water-soluble Polyamine Durable Antistatic Agent (수용성 폴리아민 내구성 대전방지제의 합성과 그의 특성화)

  • Kim, Seung-Jin;Kim, Han-Ku;Keun, Jang-Hyoun;Park, Hong-Soo
    • Applied Chemistry for Engineering
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    • v.5 no.3
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    • pp.466-477
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    • 1994
  • PEG 600-diglycidyl ethers(PDE) were synthesized using $BF_3$ catalyst by the reaction of epichlorohydrin and PEG 600 which is known to have the hygroscopicity, softening property, and antistatic property. Water-soluble long chain polyamines(PDET) were synthesized by coreaction of PDE and triethylenetetramine which is high conductive aliphatic amine curing agent. To prevent the gelation of the PDET and increase the water-solution stability, water-soluble quaternary ammonium polyamines were synthesized by cationation of PDET with acetic acid. Antistatic agents PDET-2A, PDET-5A, PDET-6A, PDETA-2A and PDETA-4A were prepared by the mixing of PDET-2, PDET-5, PDET-6, PDETA-2 and PDETA-4 with water. Synthesized antistatic agents were treated on PET textiles with and without resin. Then surface electrical resistivity and half life characteristics value were tested. As the results there were no remarkable decreasing changes in antistatic abilities of the textiles treated with PDETA-2A and PDETA-4A after 50 times washing. So PDETA-2A and PDETA-4A were proved to be durable antistatic agents. Surface electrical resistivity of the textiles treated with PDETA-2A and PDETA-4A before washing were $1{\times}10^7{\Omega}$ and $2{\times}10^7{\Omega}$, respectively, and half life characteristics values were 0.8sec and 1.1sec, respectively. Therefore PDETA-2A and PDETA-4A were proved to be good antistatic agents.

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고에너지 이온빔에 의한 고분자의 micro-hardness 특성변화

  • Choi, Han-Woo;Woo, Hyung-Joo;Hong, Wan;Kim, Gi-Dong;Kim, Jun-Gon;Kim, Young-Seok;Lee, Sam-Geun
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.112-112
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    • 1999
  • 고분자 표면에 MeV급 이온을 주입하게 되면 화학적, 광학적, 물리적, 전기적 특성 등 기존의 재래식 공정으로는 불가능한 다양한 특성변화가 일어나게 된다. 본 실험에서는 이온 조사에 따른 micro-hardness의 변화에 중점을 두어 관찰하였다. 수 MeV로 가속시킨 Cl과 C 이온을 Kapton, Teflon, PMMA에 조사량을 바꾸어가며 조사하였다. 이때 조사 전후 고분자 시료의 표면 경도는 depth-sensing nanoindentation technique (Nano Indenter II, USA)을 이용하여 측정하였다. 측정깊이는 극표면 효과와 기측효과의 영향을 무시할 수 없는 100nm로 결정하였다. 또한 이와 같은 경도변화를 규명하기 위하여 각각의 시료에 대해 FTIR, Raman, UV-VIS, RBS, XPS 스펙트럼을 측정하였으며, 조사중에 발생되는 가스상 분자들을 RGA를 이용하여 측정하였다. 1 MeV Cl 이온을 Kato에 4x1015ions/cm2 조사하면 경도가 0.35 GPa에서 7.1GPa로 약 20배 정도 증가하게 되며, 이 경도는 stainless steel 경도 2~3 GPa, martensite steel 8~12와 비교하여 보면 상당히 높은 수준임을 알 수 있다. Teflon과 PMMA 시료의 경우 1MeV Cl 이온 4X1015ions/cm2를 조사시키면 각각 경도가 0.31GPa에서 4.1a, 0.30 GPa에서 3.9GPa로 변화하였으며 Kapton에 비하여 상대적으로 경도의 변화가 적음을 알 수 있었다. 이온 주입된 Kapton의 경우 FT-IR측정에 의하여 이온 조사량이 증가함에 따라 C=O 진동, 이미드그룹의 CONH, tertiary amine의 C-N 흡수 피크가 감소되며, 1X1014ions/cm2 이상의 양이 조사되어야 개질변화가 일어남을 알 수 있었다. XPS 측정 결과 Kapton에 조사되는 이온양이 증가할수록 C=O, C-O 및 C-N의 탄소는 감소하고 페닐고리 탄소가 증가함을 알 수 있었다. 또한 이온 조사 중 측정한 RGA에서도 CO 가스가 대량 방출되는 현상을 관찰하였으며 FTIR 및 XPS에서의 C=O 결합의 감소와도 일치하였다. RBS에 의한 CNO 원소의 변화에서도 다른 원소보다 O의 감소가 현저하게 나타남을 확인하였다. UV-VIS 측정을 통해 조사 이온량에 따라 에너지 준위가 변동하여 흡수스펙트럼이 장파장으로 확대됨을 알 수 있었으며, 이는 공액 2중 결합의 형성에 의한 $\pi$-전자 및 기타 결함에 기인한다. PMMA 및 Teflon의 경우 FTIR 측정에 의하여 이온 조사됨에 따라 function group 들의 peak가 세기가 감소되면서 완만해지는 경향을 보이며 원래의 구조를 상실하게 된다. PMMA와 Teflon은 이온 조사가 되면 가교형서보다는 사슬절단이 주로 일어나므로 가교형성이 잘 일어나는 Kapton보다는 상대적으로 경도의 증가가 적음을 알 수 있었다.

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Multi-Residue Analysis of 18 Dye Residues in Animal Products by Liquid Chromatography-Tandem Mass Spectrometry

  • Park, Hyunjin;Kim, Joohye;Kang, Hui-Seung;Cho, Byung-Hoon;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.35 no.2
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    • pp.109-117
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    • 2020
  • This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL-71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C18 and primary secondary amine (PSA). Calibration linearity was obtained (r2>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.

The Study of Water Stability of MDF Cement Composite by Addition of Silane Coupling Agent (Silane Coupling Agent 첨가에 의한 MDF Cement Composite의 수분안정성 연구)

  • 노준석;김진태;박춘근;오복진;최상홀
    • Journal of the Korean Ceramic Society
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    • v.35 no.5
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    • pp.421-428
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    • 1998
  • The effect of silane coupling agents on the water stability of HAC/PVA based MDF cement composites which were modified with urethane and epoxy resin were studied as a function of the functional groups and addition amount of silane coupling agent. According to the composition of polymer matrix the silanes with different functional groups showed the different effectiveness. In case of the only PVA matrix the silane with vinyl functional group was more effective than other silanes. When the epoxy resin was added the silane of epoxy-methodxy group enhanced the flexural strength of dry and wet state more than other. In case of urethane-added MDF cement the silane of diamine group was effective and enhanced the water sta-bility fo MDF cement composite more and more as the addition amount of silane increased, Especially in case of warm-presed composite the effect of silane was enhanced By addition of 2wt% of silane with 야-amine group the flexural strength of urethane-added composites were enhanced by 20% more in dry state 40-70% in wet state in accord with the porosity analysis. The flexural strength of the poxy resin-added MDF cement composite was increased by addition of 1wt% and 2wt% silane of epoxy-methoxy group However the addition of 4wt% of silane decreased the flexural strength of dry and wet state by formation of closed pore in the polymer matrix.

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Effect of γ-Aminobutyric Acid (GABA) Producing Bacteria on In vitro Rumen Fermentation, Biogenic Amine Production and Anti-oxidation Using Corn Meal as Substrate

  • Ku, Bum Seung;Mamuad, Lovelia L.;Kim, Seon-Ho;Jeong, Chang Dae;Soriano, Alvin P.;Lee, Ho-Il;Nam, Ki-Chang;Ha, Jong K.;Lee, Sang Suk
    • Asian-Australasian Journal of Animal Sciences
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    • v.26 no.6
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    • pp.804-811
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    • 2013
  • The effects and significance of ${\gamma}$-amino butyric acid (GABA) producing bacteria (GPB) on in vitro rumen fermentation and reduction of biogenic amines (histamine, methylamine, ethylamine, and tyramine) using corn meal as a substrate were determined. Ruminal samples collected from ruminally fistulated Holstein cows served as inoculum and corn was used as substrate at 2% dry matter (DM). Different inclusion rates of GPB and GABA were evaluated. After incubation, addition of GPB had no significant effect on in vitro fermentation pH and total gas production, but significantly increased the ammonia nitrogen ($NH_3$-N) concentration and reduced the total biogenic amines production (p<0.05). Furthermore, antioxidation activity was improved as indicated by the significantly higher concentration of superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px) among treated samples when compared to the control (p<0.05). Additionally, 0.2% GPB was established as the optimum inclusion level. Taken together, these results suggest the potential of utilizing GPB as feed additives to improve growth performance in ruminants by reducing biogenic amines and increasing anti-oxidation.

Effects of Pulsed Nd:YAG Laser Irradiation and Fluoride Compound Application on Surface Hardness of Incipient Carious Lesion in Enamel of Bovine Teeth (Pulsed Nd : YAG 레이저 조사와 불소 화합물 도포가 초기 우식 법랑질의 표면 경도에 미치는 영향)

  • Jun-Bong Kwag;Woo-Cheon Kee
    • Journal of Oral Medicine and Pain
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    • v.21 no.2
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    • pp.207-224
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    • 1996
  • This study was designed to determine the most effective concentration of fluoride and energy density of laser irradiation for the anticarious effect. For this study surface hardness in enamel was measured before and after irradiation with pulsed Nd;YAG laser and the topical application of fluoride. Of the permanent mandibular anterior hovine teeth, healthy, carious free ones were used. Three hundred specimens were made. Specimens within 25~45 Vickers hardness numbers were assigned to 20 control and experimental stoops ; each containing 15 specimens. After forming artificial carious lesions, 10 J/$\textrm{cm}^2$, 20 J/$\textrm{cm}^2$, and 30 J/$\textrm{cm}^2$ energies were irradiated on the enamel surface of each experimental group. Also NaF, NH4F, Elmex gel(amine fluoride) and APF gel fluoride compounds were applied topically. Next, all the specimens were placed into the pH circulatory procedures for eight days. Vickers hardness numbers were measured using a microhardness tester. Surface changes of the enamel were observed using an scanning electron microscope. The comparative ana1ysis yielded the following results : 1. The reduction of surface hardness of the enamel surface was less in all groups with fluoride application than in the group without fluoride application. 2. The APF gel croup with 10 J/$\textrm{cm}^2$ irradiation showed the lowest reduction of surface hardness. 3. The reduction of surface hardness of the enamel surface in the group of laser irradiation without fluoride application not showed any significant difference according to the energy density of the laser. 4. Under the scanning electron microscope, in enamel irradiated with 10J/$\textrm{cm}^2$ showed appearance similar to acid etching surface. In enamel irradiated with 20 J/$\textrm{cm}^2$, line enamel crack was detected. In enamel irradiated with 30j/$\textrm{cm}^2$, severe enamel crack and fusion of enamel were detected. These results suggest that one could obtain the best anticariogenic effects without damage to teeth in the group of application of APF gel after laser irradiation with 10 J/$\textrm{cm}^2$.

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Aminopropyl Functionalized Silica Nanoparticle Dispersed Nafion Composite Membranes for Vanadium Redox Flow Batteries (아미노프로필 관능기를 갖는 실리카 나노 입자가 분산된 나피온 복합막을 이용한 바나듐 레독스 흐름 전지)

  • Lee, Doohee;Yu, Duk Man;Yoon, Sang Jun;Kim, Sangwon;So, Soonyong;Hong, Young Taik
    • Membrane Journal
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    • v.30 no.5
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    • pp.307-318
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    • 2020
  • Conventional perfluorinated sulfonic acid membrane, Nafion is widely used for vanadium redox flow battery (VRFB). It is desired to prevent vanadium ion permeation through a membrane to retain the capacity, and to keep the cell efficiency of a VRFB. Highly proton conductive and chemically stable Nafion membranes, however, suffer from high vanadium permeation, which induce the reduction in charge and discharge capacity by side reactions of vanadium ions. In this study, to resolve the issue, silica nanoparticles, which are functionalized with 3-aminopropyl group (fS) are introduced to enhance the long-term performance of a VRFB by lowering vanadium permeation. It is expected that amine groups on silica nanoparticles are converted to positive ammonium ion, which could deteriorate positively charged vanadium ions' crossover by Gibbs-Donnan effect. There is reduction in proton conductivity may due to acid-base complexation between fS and Nafion side chains, but ion selectivity of proton to vanadium ion is enhanced by introducing fS to Nafion membranes. With the composite membranes of Nafion and fS, VRFBs maintain their discharge capacity up to 80% at a high current density of 150 mA/㎠ during 200 cycles.

Heterocyclic Amines Removal by Binding Ability of Lactic Acid Bacteria Isolated from Soybean Paste (된장에서 분리된 유산균의 결합력에 의한 Heterocyclic Amines 제거)

  • Lim, Sung-Mee
    • Korean Journal of Microbiology
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    • v.50 no.1
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    • pp.73-83
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    • 2014
  • The objective of the this study was to investigate the binding capacity and removal ability of lactic acid bacterial strains obtained from Korean soybean paste for mutagenic heterocyclic amines (HCAs) formed during cooking of protein-rich food at high temperature. Among 19 strains identified by carbohydrate fermentation and 16S rRNA sequencing, the live cell or cell-free culture supernatant of Lactobacillus acidophilus D11, Enterococcus faecium D12, Pediococcus acidilactici D19, L. acidophilus D38, Lactobacillus sakei D44, Enterococcus faecalis D66, and Lactobacillus plantarum D70 inhibited the mutagenesis caused by either 3-amino-1,4-dimethyl-5H-pyrido[4,3-b] indole (Trp-P-1) or 3-amino-1-methyl-5H-pyrido[4,3-b] indole (Trp-P-2) in Salmonella typhimurium TA98 and TA100. The bacterial cells of the isolated strains showed greater binding activity than the pure cell wall, exopolysaccharide, and pepetidoglycan. The carbohydrate moieties of the cell wall or protein molecules on the cell surface have a significant role in binding Trp-P-1 and Trp-P-2, since protease, heating, sodium metaperiodate, or acidic pH treatments significantly (P<0.05) reduced the binding efficacy of the tested bacteria. Addition of metal ions or sodium dodecyl sulfate decreased the binding ability of E. faecium D12, L. acidophilus D38, and E. faecalis D66. Therefore, the binding mechanisms of these strains may consist of ion-exchange and hydrophobic bonds. Especially, the high mutagen binding by L. acidophilus D38 and L. plantarum D70 may reduce the accumulation or absorption of Trp-P-1 and Trp-P-2 in the small intestine via increased excretion of a mutagen-bacteria complex.