• 제목/요약/키워드: NMR analysis

검색결과 1,404건 처리시간 0.028초

아드만탄 기반의 새로운 설포네이트 폴리카보네이트 난연제 성능 연구 (Performance of a Novel Sulfonate Flame Retardant Based on Adamantane for Polycarbonate)

  • Guo, Jianwei;Wang, Yueqin;Feng, Lijuan;Zhong, Xing;Yang, Chufen;Liu, Sa;Cui, Yingde
    • 폴리머
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    • 제37권4호
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    • pp.437-441
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    • 2013
  • A novel sulfonate flame retardant, 1,3,5,7-tetrakis(phenyl-4-sodium sulfonate)adamantane (FR-A), was successfully synthesized from 1-bromoadamantane in sequential four-step reactions involving Fiedel-Crafts phenylation, sulphonation, hydrolysis, and neutralization. The success of synthesis was confirmed by FTIR spectra, $^1H$ NMR spectra, elemental analyses and mass spectra. The effect of FR-A on the flame retardacy of polycarbonate (PC) has been studied. Limiting oxygen index (LOI) and thermogravimetric analysis (TGA) showed that this novel sulfonate flame retardant had effective flame retardancy on polycarbonate (PC). With a small amount (0.08 wt%) of FR-A, the flame retardancy of PC was improved obviously, which got to UL 94 V-0 rating. TGA and DTA curves demonstrated that the additive raised the degradation rate of PC by promoting the quick formation of an insulating carbon layer on the surface, and confirmed that the flame retardant mechanism of PC/FR-A system was similar to potassium diphenylsulfone sulfonate (KSS).

Cytotoxic and ACAT-inhibitory Sesquiterpene Lactones from the Root of Ixeris dentata forma albiflora

  • Ahn, Eun-Mi;Bang, Myun-Ho;Song, Myoung-Chong;Park, Mi-Hyun;Kim, Hwa-Young;Kwon, Byoung-Mog;Baek, Nam-In
    • Archives of Pharmacal Research
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    • 제29권11호
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    • pp.937-941
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    • 2006
  • Ixeris dentata forma albiflora was extracted with 80% aqueous MeOH, and the concentrated extract was partitioned with EtOAc, n-BuOH and $H_{2}O$. Eight sesquiterpenes were isolated through repeated silica gel and octadecyl silica gel ($C_{18},\;ODS$) column chromatography of the EtOAc and n-BuOH fractions. Physicochemical analysis using NMR, MS and IR revealed the chemical structures of the sesquiterpenes, which were zaluzanin (1), 9a-hydroxyguaian-4(15), 10(14), 11 (13)-triene-6, 12-olide(2), $3{\beta}-O-{\beta}-D-glucopyranosyl-8{\beta}-hydroxyguaian$-4(15), 10(14)-diene-6, 12-olide (3), $3-O-{\beta}-D-glucopyranosyl-8{\beta}-hydroxyguauan$-10(14)-ene-6, 12-olide (4), ixerin M (5), glucozaluzanin C (6), crepiside I (7), and ixerin D (8). This is the first time that these sesquiterpene lactones have been isolated from this plant. Compounds 1, 2 and 7 revealed relatively high cytotoxicities on human colon carcinoma cell and lung adeno-carcinoma cell, while compounds 5 and 7 showed acyl-CoA: cholesterol acyltransferase (ACAT) inhibitory activity.

약물방출시스템 적용을 위한 락타이드/히아루론산 고분자 막의 제조 (Synthesis of Lactide/Hyaluronic Acid Polymer Membrane for the Application of Drug Delivery System)

  • 김민수;권지영;정성일
    • 멤브레인
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    • 제15권4호
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    • pp.281-288
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    • 2005
  • 생체 적합성이 우수한 히아루론산과 생분해성이 우수한 폴리 락타이드의 이량체를 결합하여 약물 방출 시스템에 적용할 수 있는 생체 재료를 제조하고자 하였다. 냉동 건조법을 이용하여 히아루론산과 락타이드를 가교제 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC)로 가교시켰다. 생성된 막을 핵자기 공명 분광법으로 분석하여 락타이드 반응도와 EDC 반응도를 결정하였다. 히아루론산에 대한 락타이드 몰비, 가교제 농도가 증가할수록 혹은 가교 온도가 감소할수록, 락타이드 반응도가 증가하였으며 팽윤도는 감소하였다. 서로 다른 락타이드 반응도를 가진 막으로 약물 방출 실험을 수행한 결과 락타이드 반응도가 증가하면 약물 방출 속도가 감소하는 경향을 보였다. 또 친수성이 다른 여러 가지 약물로 약물 방출 실험을 수행한 결과 친수성이 우수한 약물일수록 서서히 방출되었다.

Methacrylamidohistidine in Affinity Ligands for Immobilized Metal-ion Affinity Chromatography of Human Serum Albumin

  • Odaba, Mehmet;Garipacan, Bora;Dede, Semir;Denizli, Adil
    • Biotechnology and Bioprocess Engineering:BBE
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    • 제6권6호
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    • pp.402-409
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    • 2001
  • Different bioligands carrying synthetic adsorbents have been reported in the literature for protein separation, We have developed a novel and new approach to obtain high protein ad-sorption capacity utilizing 2-methacrylamidohistidine(MAH) as a bioligand. MAH was synthe-sized by reacting methacrylocholride and histidine, Spherical beads with an average size of 150-200㎛ were obtained by the radical suspension polymerization of MAH and 2-hydrosyethyl-methacrylate(HEMA) conducted in an aqueous dispersion medium. p(HEMA-co-MAH) beads had a specific surface area of 17.6㎡/g . Synthesized MAH monomer was characterized by NMR. p(HEMA-co-MAH) beads were characterized by swelling test, FTIR and elemental analysis. Then Cu(II) ions were incorporated onto the beads and Cu(II) loading was found to be 0.96 mmol/g.These affinity beads with a swelling ration of 65% and containing, 1.6 mmol MAH/g were used in the adsorption/desorption of human serum albumin(HSA) from both aqueous solutions and hu-man serum. The adsorption of HSA onto p(HEM-co-MAH) was low(8.8 mg/g). Cu(II) chelation onto the beads significantly increased the HSA adsorption (56.3 mg/g). The maximum HSA ad-sorption ws observed at pH 8.0 Higher HSA adsorption was observed from human plasma(94.6 mgHSA/g) Adsorption of other serum proteins were obtained as 3.7 mg/g for fibrinogen and 8.5mg/g for γ-globulin. The total protein adsorption was determined as 107.1mg/g. Desorption of HSA was obtained using 0.1 M Tris/HCl buffer containing 0.5 M NaSCN, High desorption rations(up to 98% of the adsorbed HSA) were observed. It was possible to reuse Cu(II) chelated-p(HEMA-co-MAH) beads without significant decreases in the adsorption capacities.

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유산균 발효에 의한 소청룡탕의 발효 전 후 성분 변화 연구 (Analysis of Constituents in Socheongryong-tangs Fermented by Lactic acid bacteria)

  • 양민철;김동선;정상원;마진열
    • 한국한의학연구원논문집
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    • 제17권3호
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    • pp.115-121
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    • 2011
  • Objective : The purpose of this study was to investigate the changes in the contents of constituents in Socheongryong-tang (CY) and its fermentations (FCY) with 10 species of lactic acid bacteria. Methods : Ten strains of lactic acid bacteria, Lactobacillus casei 127, L. acidophilus 128, L. casei 129, L. plantarum 144, L. amylophilus 161, L. curvatus 166, L. delbruekil subsp. lactis 442, L. casei 693, B. breve 744, and B. thermophilum 748, were used for the fermentation of Socheongryong-tang. The increased and decreased constituents were identified using HPLC/DAD and various liquid chromatographic techniques, and the structure was elucidated using NMR and MS. These compounds were quantitatively analyzed using an HPLC/DAD system. Results : The increased constituents were identified to be liquiritigenin (1) and cinnamyl alcohol (2), and the decreased constituent was determined to be liquiritin (3). Liquiritigenin (1) and cinnamyl alcohol (2) were increased in all of the FCYs, while liquiritin (3) was decreased. The fermentation of the ten lactic acid bacteria demonstrated that the decomposable rate of these three compounds in FCYs were different. Socheongryong-tang fermented by L. plantarum 144 and L. amylophilus 161 showed the most remarkable changes. Conclusions : CY could be increased antibacterial, neuroprotective, or antiinflammatory effect by fermentation with lactic acid bacteria, especially with L. plantarum and L. amylophilus, considering their known biological activities. In addition, it is expected that this study will help to establish quality control parameters for FCY.

Swallow-Tail Terrylene Bisimide 적색 유기 형광체 제조 및 특성 연구 (Preparation and Characterization of Swallow-Tail Terrylene Bisimide as Organic Phosphor)

  • 정성봉;정연태
    • 한국전기전자재료학회논문지
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    • 제33권3호
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    • pp.194-200
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    • 2020
  • Perylene bisimide derivatives are developed for red organic phosphor because of their advantages, such as excellent luminous efficiency and high thermal stability. Despite these advantages, they have poor solubility characteristics in organic solvents and short emission wavelength as red organic phosphor for hybrid light-emitting diodes (LEDs). In this study, we prepared terrylene bisimide using a coupling reaction and swallow-tail imide group, which has excellent solubility. The structures and properties of swallow-tail terrylene bisimide (9C) were analyzed using 1H-nuclear magnetic resonance (1H-NMR), Fourier-transform infrared (FT-IR), UV/Vis spectroscopy, and thermal gravimetric analysis (TGA). The maximum absorption wavelength of (9C) in the UV/Vis spectrum was 647 nm, and the maximum emission wavelength was 676 nm. In the TGA, (9C) demonstrated good thermal stability with less than 5 wt% weight loss up to 415℃. In the solubility test, (9C) has a good solubility of more than 5 wt% in chloroform and dichloromethane. When the compounds (9C) were mixed with PMMA (polymethly methacrylate), the films showed peaks at 680 nm in the PL spectra. The results verify the suitability of (9C) as a red organic phosphor for hybrid LEDs.

RGD-Conjugated Chitosan-Pluronic Hydrogels as a Cell Supported Scaffold for Articular Cartilage Regeneration

  • Park, Kyung-Min;Joung, Yoon-Ki;Park, Ki-Dong;Lee, Sang-Young;Lee, Myung-Chul
    • Macromolecular Research
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    • 제16권6호
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    • pp.517-523
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    • 2008
  • A RGD (Arg-Gly-Asp) conjugated chitosan hydrogel was used as a cell-supporting scaffold for articular cartilage regeneration. Thermosensitive chitosan-Pluronic (CP) has potential biomedical applications on account of its biocompatibility and injectability. A RGD-conjugated CP (RGD-CP) copolymer was prepared by coupling the carboxyl group in the peptide with the residual amine group in the CP copolymer. The chemical structure of RGD-CP was characterized by $^1H$ NMR and FT IR. The concentration of conjugated RGD was quantified by amino acid analysis (AAA) and rheology of the RGD-CP hydrogel was investigated. The amount of bound RGD was $0.135{\mu}g$ per 1 mg of CP copolymer. The viscoelastic parameters of RGD-CP hydrogel showed thermo-sensitivity and suitable mechanical strength at body temperature for cell scaffolds (a> 100 kPa storage modulus). The viability of the bovine chondrocyte and the amount of synthesized glycosaminoglycans (GAGs) on the RGD-CP hydrogels were evaluated together with the alginate hydrogels as a control over a 14 day period. Both results showed that the RGD-CP hydrogel was superior to the alginate hydrogel. These results show that conjugating RGD to CP hydro gels improves cell viability and proliferation, including extra cellular matrix (ECM) expression. Therefore, RGD conjugated CP hydrogels are quite suitable for a chondrocyte culture and have potential applications to the tissue engineering of articular cartilage tissue.

Investigation of Siderophore production and Antifungal activity against Phytophthora capsici as related to Iron (III) nutrition by Lysobacter antibioticus HS124

  • Ko, Hyun-Sun;Tindwa, Hamisi;Jin, Rong De;Lee, Yong-Seong;Hong, Seong-Hyun;Hyun, Hae-Nam;Nam, Yi;Kim, Kil-Yong
    • 한국토양비료학회지
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    • 제44권4호
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    • pp.650-656
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    • 2011
  • Lysobacter antibioticus HS124 isolated from pepper rhizosphere soil produced catechol type siderophore. Purified siderophore by Diaion HP-20 and silica gel column chromatography showed several hydroxyl functional groups adjacent to benzene rings by analysis of $^1H$ NMR spectroscopy. The strain HS124 showed different activities to suppress Phytophthora capsici with different concentrations of exogenous Fe (III) in minimal medium where antifungal activity with $100{\mu}M$ Fe (III) was approximately 1.5 times higher than in absence of Fe (III). Bacterial population in this Fe (III)-amended medium was also highest with $8.9{\times}10^8\;CFU\;ml^{-1}$ which also corresponded to the strongest siderophore activity. When grown in rich medium (minimal medium with N, $P_2O_5K_2O$ and glucose), HS124 exhibited approximately 2 times stronger antifungal activity compared to minimal medium. In pot trials, treatments of bacterial culture grown in rich medium with (C1) or without (C2) $100{\mu}M$ Fe (III) exhibited a high protection of pepper plants from disease, compared to medium only with (M1) or without (M2) $100{\mu}M$ Fe (III). Especially, treatment C1 showed the best disease control effect of about 70 %. Thus, the strain HS124 should be recommended as a potential biocontrol agent against P. capsici in pepper.

부신수실 영상용 $^{131}I$ 표지 메타요오도벤질구아니딘 $(^{131}I-MIBC)$의 제조에 관한 연구 (Studies on Preparation of $^{131}I$ Labelled m-Iodobenzylguanidine $(^{131}I-MIBG)$ for Adrenomedullary Imaging)

  • 박경배;오옥두;김재록
    • 대한핵의학회지
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    • 제24권1호
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    • pp.101-107
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    • 1990
  • To develop $^{131}I-labelled$ m-iodobeneylguanidine $(^{131}I-MIBG)$, various experiments such as synthesis of MIBG, establishment of labelling conditions, determination of radiochemical purity, and examination of stability were carried out. 1) m-Iodobenzylguanidine (MIBG) sulfate was synthesized with a total yield of 62.4% by the condensation of m-iodobenzylamine hydrochloride with cyanamide via MIBG bicarbonate. Its physical properties, IR, $^1H-NMR$, and elemental analysis data were nearly identical to those of literature. 2) Freeze-dried or vacuum-dried kit vials were prepared from the mixture so as to contain MIBG (2 mg), ascorbic acid (10 mg), copper (II) sulfate (0.14 mg), and tin (II) sulfate (0.5 mg) per vial. Copper ( I ) catalyzed radioiodination of MIBG was carried out using kit vials and 0.01 M $H_2SO_4$ as solvent at $100^{\circ}C$ for 30 min under nitrogen atmosphere (optimal conditions). Labelling yield was 98% and radiochemical purity was 99.5%, respectively. 3) Solid-phase radioiodination of MIBG was carried out at $155^{\circ}C$ for 30 min using the prepared vials to contain MIBG (2 mg) and ammonium sulfate (10 mg). Duplicate reactions under the same conditions showed labelling yield of 95% and radiochemical purity of 99.5%. 4) $^{131}I-MIBG$ prepared either by catalytic or by solid-phase exchange method showed radio-chemical purity of 99% even after 3 days storing at room temperature.

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수종 복합레진 내의 bis-GMA와 TEGDMA의 구성비가 레진 인레이 법에 의한 부가적 열처리시 복합레진의 표면 및 내부의 중합률 변화에 미치는 영향 (CORRELATION BETWEEN BIS-GMA : TEGDMA RATIO AND DEGREE OF CONVERSION IN VARIOUS LAYERS OF COMPOSITE AFTER ADDITIONAL HEAT CURING)

  • 박성호;정찬문
    • Restorative Dentistry and Endodontics
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    • 제21권2호
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    • pp.642-651
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    • 1996
  • The purpose of this study was to evaluate the relationship between monomer compositions and the changes in the degree of conversion in the various layers of composites after additional heat curing. Four types of composites and 3 types of inlay ovens were used in this study. Composite was placed in a 4-mm thick teflon mold, and light cured from the top for 60 seconds. Ten samples were prepared for each composite ; 5 of these were additionally heat cured in an inlay oven as the manufacturer recommended. After light curing or light and heat curing, the samples were sectioned into four parts and assigned to groups A, B, C, or D according to their distance from the light source. These sections were then thinned to 50-$70{\mu}m$, and these wafers were analyzed with a Fourier Transform Infrared Spectrometer(FI-IR) to determine the degree of conversion. A standard baseline technique was used to calculate the degree of conversion. $^{13}C$ NMR spectra of bis-GMA, TEGDMA and bis-EMA, were acquired using a Varian Gemini spectrometer operated at 200 MHz. $CDCl_3$ solvent was used for qualitative analysis. The degree of conversion was affected by bis-GMA : TEGDMA ratio but it seemed to be also affected by other factors. When the composites were heat cured, significant increases in the degree of conversion were noted throughout the samples, but the amount of increase differed between materials. Thus, clinical performance of a heat-treated composite inlay may be different depending on materials.

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