• Title/Summary/Keyword: $^{1}H$ NMR

Search Result 2,515, Processing Time 0.03 seconds

A detailed study of physicochemical properties and microstructure of EmimCl-EG deep eutectic solvents: Their influence on SO2 absorption behavior

  • Zhu, Jiahong;Xu, Yingjie;Feng, Xiao;Zhu, Xiao
    • Journal of Industrial and Engineering Chemistry
    • /
    • v.67
    • /
    • pp.148-155
    • /
    • 2018
  • To get a better understanding of the effect of physicochemical properties and microstructure on $SO_2$ absorption behavior of DESs with different molar ratios of EmimCl and EG (from 2:1 to 1:2), densities (${\rho}$), viscosities (${\eta}$), speeds of sound (u), refractive indices ($n_D$), and thermal decomposition temperatures ($T_d$) of EmimCl-EG DESs were measured and used to obtain the other derived properties, such as thermal expansion coefficient (${\alpha}_p$) and activation energy for viscous flow ($E_{\eta}$). Moreover, FT-IR spectra and in situ variable-temperature NMR spectroscopy were employed to study the microstructures of DESs. Based on physicochemical and spectroscopic properties, the influence of the concentrations of EmimCl on the interactions in DESs was explored to be associated with their $SO_2$ absorption behavior. The results show that the interactions between $Emim^+$ and $Cl^-$ of EmimCl is gradually weakening with increasing the concentration of EG in DESs by forming of hydrogen bond interaction of $O-H{\cdots}Cl^-$, resulting in a decrease of ${\rho}$, ${\eta}$, u, $n_D$, and $T_d$ of DESs, and hindering the charge-transfer interaction of $SO_2$ with $Cl^-$ and deceasing $SO_2$ capture capacity. Moreover, the $SO_2$ absorption capacity of DESs is proportional to their ${\rho}$ and $E_{\eta}$, respectively.

Studies on Biological Activity of Wood Extractives (X) - Antifungal Compounds of Hovenia dulcis - (수목추출물의 생리활성에 관한 연구(X) - 헛개나무 목부의 항균활성 물질 -)

  • Choi, Yun-Jeong;Lee, Hak-Ju;Lee, Sung-Suk;Choi, Don-Ha
    • Journal of the Korean Wood Science and Technology
    • /
    • v.31 no.1
    • /
    • pp.1-9
    • /
    • 2003
  • Antimicrobial activities of plant extractives were investigated to develop a natural fungicide. Two stilbenoids and five flavonoids were isolated from wood extractives of Hovenia dulcis (Rhamnaceae) which had been selected due to its high antifungal activity among the tested species. The chemical structures of isolated compounds were determinded as : 5-hydroxy-7-methoxyflavone, 5,7-dihydroxyflavone (chrysin), 5,7-dihydroxyflavanone (pinocembrin), 3,5,7-trihydroxyflavanone (pinobanksin), 3,4',5,7-tetrahydroxyflavanone (aromadendrin), 3-hydroxy-5-methoxystilbene and 3,5-dihydroxystilbene (pinosylvin) on the basis of Mass and NMR spectroscopic data. According to the results of antifungal test, 3-hydroxy-5-methoxystilbene was evaluated as the strongest antifungal compound among the tested compounds and next were pinocembrin and pinosylvin, but those also had high hyphal growth inhibition activities against C. parasitica, T. versicolor, T. palustris and T. viride. However, pinobanksin, 5-hydroxy-7-methoxyflavone, chrysin and aromadendrin showed very low antifungal activity. In this regard, it could inferred that high antifungal activity of wood extractives of H. dulcis were derived from 3-hydroxy-5-methoxystilbene, pinocembrin and pinosylvin, respectively.

Multi-Function of a New Bioactive Secondary Metabolite Derived from Endophytic Fungus Colletotrichum acutatum of Angelica sinensis

  • Ramy S. Yehia
    • Journal of Microbiology and Biotechnology
    • /
    • v.33 no.6
    • /
    • pp.806-822
    • /
    • 2023
  • In the current study we assessed a new crystallized compound, 5-(1-hydroxybutyl)-4-methoxy-3-methyl-2H-pyran-2-one (C-HMMP), from the endophytic fungus Colletotrichum acutatum residing in the medicinal plant Angelica sinensis for its in vitro antimicrobial, antibiofilm, antioxidant, antimalarial, and anti-proliferative properties. The promising compound was identified as C-HMMP through antimicrobial-guided fraction. The structure of C-HMMP was unambiguously confirmed by 2D NMR and HIRS spectroscopic analysis. Antimicrobial property testing of C-HMMP showed it to be effective against a variety of pathogenic bacteria and fungi with MICs ranging from 3.9 to 31.25 ㎍/ml. The compound displayed excellent antibiofilm activity against C. albicans, S. aureus, and K. pneumonia. Furthermore, the antimalarial and radical scavenging activities of C-HMMP were clearly dosedependent, with IC50 values of 0.15 and 131.2 ㎍/ml. The anti-proliferative activity of C-HMMP against the HepG-2, HeLa, and MCF-7 cell lines in vitro was investigated by MTT assay, revealing notable anti-proliferative activity with IC50 values of 114.1, 90, and 133.6 ㎍/ml, respectively. Moreover, CHMMP successfully targets topoisomerase I and demonstrated beneficial anti-mutagenicity in the Ames test against the reactive carcinogenic mutagen, 2-aminofluorene (2-AF). Finally, the compound inhibited the activity of α-glucosidase and α-amylase with IC50 values of 144.7 and 118.6 ㎍/ml, respectively. To the best of our knowledge, the identified compound C-HMMP was obtained for the first time from C. acutatum of A. sinensis, and this study demonstrated that C-HMMP has relevant biological significance and could provide better therapeutic targets against disease.

Isolation and quantitative analysis of metabolites from Scrophularia buergeriana and their hepatoprotective effects against HepG2 Cells (현삼 (Scrophularia buergeriana)에서 분리한 화합물의 함량분석 및 간세포 보호 효과)

  • Na, Hyeon Seon;Oh, Seon Min;Shin, Woo Cheol;Bo, Jeon Hwang;Kim, Hyoung-Geun;Yoon, Dahye;Yang, Seung Hwan;Lee, Young-Seob;Kim, Geum-Soog;Baek, Nam-In;Lee, Moon-Soon;Lee, Dae Young
    • Journal of Applied Biological Chemistry
    • /
    • v.62 no.4
    • /
    • pp.399-406
    • /
    • 2019
  • The roots of Scrophularia buergeriana were extracted with 80% aqueous Methanol and the concentrates were partitioned into EtOAc, n-BuOH, and H2O fractions. The repeated silica gel or octadecyl SiO2column, and medium pressure liquid chromatographies for the n-BuOH fraction led to isolation of phenylethanoid glycosides and iridoid glycosides. The chemical structures of these compounds were determined as harpagoside (1), angoroside C (2), aucubin (3) and acetoside (4) based on spectroscopic analyses including nuclear magnetic resonance and MS. A simple and efficient HPLC with UV detection method for the simultaneous determination of the four compounds (1-4) has been developed and applied to their content determination in the S. buergeriana. The roots were extracted by 80% methanol, and the contents of 1, 2, 3, and 4 were determined to 11.5, 7.6, 41.2, and 4.8 mg/g, respectively. Additionally, angoroside C (2) and acetoside (4) exhibited hepatoprotective effect against ethanol-induced hepatotoxicity in HepG2 cell line.

Studies on the Determination Method of Monascus Pigments in Foods (식품 중 홍국색소의 분석법에 관한 연구)

  • Lee, Tal-Soo;Lee, Young-Ja;Kwon, Yong-Kwan;Park, Jae-Seok;Ko, Hyun-Sook;Sim, Kyu-Chang;Lee, Ju-Yeun;Shin, Jae-Wook;Song, Jee-Won;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
    • /
    • v.33 no.5
    • /
    • pp.641-644
    • /
    • 2001
  • This study was performed for development of new analytical method of monascus pigments in foods. In this method, analysis of monascus pigment in foods has been carried out by detection of monascin and ankaflavin of the main color component of monascus pigment as indicator compounds. Monascin and ankaflavin were isolated and identified by TLC, HPLC, Prep. HPLC, $^{1}H-NMR$ and Mass spectrophotometer. The analysis of monascin and ankaflavin in foods such as massal, sausage, mixed press ham, mixed fish sausage, semi-dried sausage and syrup was performed by using reverse phase high performance liquid chromatograph with Capcell Pak C18 column at wave length 390 nm. The quantitative results of monascin were as follows : $0.01{\sim}3.31\;{\mu}g/g$ item in massal, $0.05{\sim}0.10\;{\mu}g/g$ in mixed fish sausage, and $0.34{\sim}0.35\;{\mu}g/g$ in semi-dried sausage. But the quantitative results of ankaflavin were as follows: $0.02{\sim}0.89\;{\mu}g/g$ in massal, ankaflavin were not founded in other samples.

  • PDF

Synthesis of Aluminophosphate using Structure Directing Agent containing Piperidine Moiety: Effect of SDA on Crystal Structure (피페리딘 구조유도분자를 이용한 알루미노포스페이트 제올라이트 합성: 피페리딘 구조유도분자가 결정구조 형성에 미치는 영향)

  • Shin, Hye Sun;Jang, Ik Jun;Shin, Na Ra;Ju, Bit Na;Cho, Sung June
    • Korean Chemical Engineering Research
    • /
    • v.49 no.5
    • /
    • pp.657-663
    • /
    • 2011
  • Structure directing agent(SDA) containing piperidine moiety such as piperidine(PI), 2-methylpiperidine (MPI), 2,6-dimethylpiperidine(DMPI) and 2,2,6,6,-tetramethylpiperidine(TMPI), respectively has been utilized to synthesize aluminophosphate zeolite using hydrothermal method. The gel composition was $1.0Al_2O_3:1.0P_2O_5:0.76SDA:45H_2O$ and the hydrothermal heating was performed in an oven at 443 K and for 7 days at static mode. The obtained zeolitic material contained a lamellar structure when PI was used as the SDA. With a progressive increase of the SDA size, various structures of aluminophosphate including AlPO-5 of AFI structure were obtained. The aluminophosphate of SAS structure was formed when the largest TMPI was utilized as the SDA, which was confirmed by the Rietveld refinement. The result of $^{27}Al$ and $^{31}P$ MAS NMR of the sample suggested that Al and P were incorporated into the framework of the aluminophosphate.

버섯의 항암효과 -영자 균사체 다당류의 항종양 활성-

  • 이준우
    • Proceedings of the Korean Journal of Food and Nutrition Conference
    • /
    • 1997.06b
    • /
    • pp.13-14
    • /
    • 1997
  • 영지의 약리효과는 triterpenoid계의 저분자와 polysaccharide인 고분자로 대별할 수 있다. 저분자 물질은 항염증작용, 항알러지작용, 간암세포 성장 억제작용, 혈압 강하작용, 혈소판 응집저해작용 등이 있으며, 고분자 물질은 혈압강하작용, 정혈작용, 고지혈증 개선작용, 혈당 강하작용, 면역 증강작용 및 항종양작용 등이 있는 것으로 알려졌다. 현재까지의 영지에 관한 연구는 주로 자실체에 대한 연구가 주류를 이루고 있으며 이들의 산지, 환경조건, 채집시기 및 실험자들에 따라 약리 효과 등에 많은 차이가 있다. 이들에 대한 효과가 영지의 대표적 약리효과라고 언급하기엔 부족한 점이 많으므로 약리효과가 우수하고 일관성이 있는 영지 유래 다당류를 얻기 위한 방법으로서는 균사체의 대량배양법 및 분리방법이 확립 되어야만 한다. 본 연구에서는 새로운 항암활성 다당류의 개발을 위해 국내 자생 영지를 채집하여 검색 및 계통적 분류를 행하였으며 분리된 균주의 최적 액체배양 조건, 다당류 분리 조건, 다당류의 물리화학적 특성 및 약리활성 등에 관한 연구를 실시하였다. 그 중 약리활성이 우수한 G- lucidum IY009 균주를 선발 하였다. 구조적 특징과 종양 면역 활성과의 관계 규명을 위해, G- lucidum IY009 배양균사체로부터 다당류를 T-AS, U-AS, M-AS, S 및 H로 분획 하였다. 추출조건에 따른 다당류 GLG의 수율은 열수 추출 분획이 2.98g/l로 가장 높았으며, U-AS및 T-AS에서 각각 2.32g/l, 2.07g/l이었다. GLG의 특성을 조사하기 위하여 수용성과 비수용성으로 분리한 결과 수용성 분획은 비수용성 분획보다 높은 당 함량을 나타냈으며, T-AS는 70.3%의 당과 7.8%의 단백질로 구성 되었다. GLG 대부분의 분획들은 60~93%의 glucose로 구성된 다당류 이었으며, 주로 $\beta$-glucose로 구성된 다당류 이었다. 아미노산은 Asp 및 Glu의 산성 아미노산과 Ala, Leu 등의 함량이 높게 나타났으며, 비알칼리 추출물에서 Ser과 Thr의 함량이 높게 나타났다. 다당류 T-AS는 평균 분자량이 2,000 kD와 12kD에서 주 peak를 나타냈으며, 수용성 분획의 평균 분자량은 12kD이고 비수용성 분획은 36~2,000 kD의 평균 분자량 분포를 갖는 것으로 나타났다. IR과 NMR 분석 결과 890 cm-1에서 흡수 peak를 나타내어 $\beta$-(1,3)0glucan과 $\beta$-(1,6)-glucan의 구조를 갖는 다당류로 확인 되었다. T-AS 분획은 C:H:O:N의 함량비가 38.9:5.7:49.6:1.84%이며, 이 물질의 융점은 163 $^{\circ}C$로 연한 갈색을 나타낸다. 분리된 GLG의 항암활성 기전 규명을 위해, in vivo 항암실험, 항보체 활성능, 항체 생성능, serum protein 분비능, 대식세포의 탐식능과 활성능 및 세포간 물질 분비 등의 상관관계를 조사하였다. 다당류 GLG 분획물들 가운데 항보체의 활성이 높았던 분획은 sarcome 180에 대한 항암 활성이 높게 나타났다. 다당류 T-AS의 보체 활성화 기작은 classical과 alternative complement pathway의 양 경로를 통해 활성화 되었다. T-AS 분획은 mouse내의 특정 혈청단백을 증가시켰으며, 항체 생성능의 증가가 관찰되어 effect T 세포의 활성화가 나타나고 있음을 알 수 있었다. T-AS는 생체내 투여시에 대식세포의 탐식능이 증진되었으며, 대식세포 기능 저해제에 의한 대식세포의 기능 저해 현상이 회복되었다. 이와 같은 결과들로부터, T-AS의 항암 활성은 활성화된 보체 성분 및 당 수용체들이 존재하는 대식세포의 개입을 시사한다.

  • PDF

Structural Analysis of the Unusual Sugar-Containing Oligosaccharides Formed by the Selective Cleavage of Weakly Acidic Polysaccharide (약산성 다당의 선택적 분해 과정에서 얻어진 특이당 함유 Oligo당의 구조적 분석)

  • Shin, Kwang-Soon;Lee, Ho
    • Korean Journal of Food Science and Technology
    • /
    • v.29 no.6
    • /
    • pp.1105-1112
    • /
    • 1997
  • By sequential degradation using partial acid hydrolysis of a weakly acidic polysaccharide (GL-4IIb2'), two acidic oligosaccharide fragments, PA-2' and PA-1-III were isolated and their structures were characterized. PA-2' consisted of almost equal proportion of a rhamnose (Rha) and an unusual sugar, 3-deoxy-D-manno-2-octurosonic acid (Kdo). When permethylated oligosaccharide-alditol derived from PA-2' was analyzed by GC-MS, the peak gave the fragment ions at m/z 189 $(bA_1,\;6-deoxyhexose)$ and at m/z 308 $(aJ_2,\;alditol\;from\;Kdo)$. The peak also gave the characteristic ion at m/z 162 but it did not give the fragment ion at m/z 177, suggesting that Kdo is substituted at C5 but not at C4. Methylation analysis also indicated that PA-2' was composed mainly of terminal Rhap and 5-substituted Kdo. When the reduced product from PA-2' was analyzed by $^1H-NMR$, it gave a signal at 5.09 ppm due to an anomeric proton of ${\alpha}-L-Rha$. These results indicated that PA-2' mainly contained ${\alpha}-L-Rhap-(1{\rightarrow}5)-Kdo$. On the other hand, PA-1-III mainly comprised Rha and Kdo in addition to small proportions of arabinose (Ara) and 3-deoxy-D-lyxo-2-heptulosaric acid (Dha). MS analysis of permethylated oligosaccharide-alditols from PA-1-III suggested that the major peak 1P was $Rhap-(1{\rightarrow}5)-Kdo$ whereas the minor peaks 2P and 3P possessed $Araf-(1{\rightarrow}5)-Dha$ unit and these peaks were produced as epimers during reduction of carbonyl groups in Dha.

  • PDF

The Effect of Nuclear Overhauser Enhancement in Liver and Heart $^{31}P$ NMR Spectra Localized by 2D Chemical Shift Technique (이차원 화학변위 기법을 이용한 간 및 심장 $^{31}P$ 자기공명분광에서의 Nuclear Overhauser 효과에 대한 연구)

  • Ryeom Hun-Kyu;Lee Jongmin;Kim Yong-Sun;Lee Sang-Kwon;Suh Kyung-Jin;Bae Sung-Jin;Chang Yongmin
    • Investigative Magnetic Resonance Imaging
    • /
    • v.8 no.2
    • /
    • pp.94-99
    • /
    • 2004
  • Purpose : To investigate the signal enhancement ratio by NOE effect on in vivo $^{31}P$ MRS in human heart muscle and liver. we also evaluated the enhancement ratios of different phosphorus metabolites, which are important in 31P MRS for each organ. Materials and Methods : Ten normal subjects (M:F = 8:2, age range = 24-32 yrs) were included for in vivo $^{31}P$ MRS measurements on a 1.5 T whole-body MRI/MRS system using $^1H-^{31}P$ dual tuned surface coil. Two-dimensional Chemical Shift Imaging (2D CSI) pulse sequence for $^{31}P$ MRS was employed in all $^{31}P$ MRS measurements. First, $^{31}P$ MRS performed without NOE effect and then the same 2D CSI data acquisitions were repeated with NOE effect. After postprocessing the MRS raw data in the time domain, the signal enhancements in percent were estimated from the major metabolites. Results : The calculated NOE enhancement for liver $^{31}P$ MRS were $\alpha-ATP\;(7\%),\;\beta-ATP\;(9\%),\;\gamma-ATP\;(17\%),\;Pi\;(1\%),\;PDE\;(19\%)$ and $PME\;(31\%)$. Because there is no creatine kinase activity in liver, PCr signal is absent. For cardiac $^{31}P$ MRS, whole body coil gave better scout images and thus better localization than surface coil. In $^{31}P$cardiac multi-voxel spectra, DPG signal increased from left to right according to the amount of blood included. The calculated enhancement for cardiac $^{31}P$ MRS were : $\alpha-ATP\;(12\%),\;\beta-ATP\;(19\%),\;\gamma-ATP\;(30\%),\;PCr\;(34\%),\;Pi\;(20\%),\;(PDE)\;(51\%),\;and\;DPG\;(72\%)$. Conclusion : Our results revealed that the NOE effect was more pronounced in heart muscle than in liver with different coupling to 1H spin system and thus different heteronuclear cross-relaxation.

  • PDF

Data Mining Approaches for DDoS Attack Detection (분산 서비스거부 공격 탐지를 위한 데이터 마이닝 기법)

  • Kim, Mi-Hui;Na, Hyun-Jung;Chae, Ki-Joon;Bang, Hyo-Chan;Na, Jung-Chan
    • Journal of KIISE:Information Networking
    • /
    • v.32 no.3
    • /
    • pp.279-290
    • /
    • 2005
  • Recently, as the serious damage caused by DDoS attacks increases, the rapid detection and the proper response mechanisms are urgent. However, existing security mechanisms do not effectively defend against these attacks, or the defense capability of some mechanisms is only limited to specific DDoS attacks. In this paper, we propose a detection architecture against DDoS attack using data mining technology that can classify the latest types of DDoS attack, and can detect the modification of existing attacks as well as the novel attacks. This architecture consists of a Misuse Detection Module modeling to classify the existing attacks, and an Anomaly Detection Module modeling to detect the novel attacks. And it utilizes the off-line generated models in order to detect the DDoS attack using the real-time traffic. We gathered the NetFlow data generated at an access router of our network in order to model the real network traffic and test it. The NetFlow provides the useful flow-based statistical information without tremendous preprocessing. Also, we mounted the well-known DDoS attack tools to gather the attack traffic. And then, our experimental results show that our approach can provide the outstanding performance against existing attacks, and provide the possibility of detection against the novel attack.