• 제목/요약/키워드: High-resolution mass spectrometry

검색결과 122건 처리시간 0.021초

Flavonol Glycosides with Antioxidant Activity from the Aerial Parts of Epimedium koreanum Nakai

  • Kim, Eun-Sil;Kim, Mi-Kyung;Kang, Hyun-Kyu;Park, Young-In;Dong, Mi-Sook;Kim, Dong-Hyun;Chung, Ha-Sook
    • Natural Product Sciences
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    • 제14권4호
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    • pp.233-238
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    • 2008
  • The aerial parts of Epimedium koreanum Nakai have been used to stimulate hormone secretion in treating impotence. Ten flavonol glycosides, 3,4,5-trihydroxy-8-prenylflavone 7-O-[${\beta}$-D-glucopyranosyl($1{\rightarrow}2$)-${\beta}$-D-glucopyranoside] (1), hyperoside (2), icarisid II (3), 2"-O-Rhamnosylicarisid II (4), epimedin A (5), epimedin B (6), epimedin C (7), icariin (8), hexandraside E (9), and epimedoside A (10) were isolated from the an ethylacetate soluble extracts of the aerial parts of Epimedium koreanum Nakai through activity-monitord fractionation and isolation method. The structures of compounds 1 - 10 were elucidated by high resolution fast atom bombardment mass spectrometry and two dimentional nuclear magnetic resonance spectroscopy analysis. Compounds 1 and 4 showed potent antioxidant activity, with $IC_{50}$ values of 19.7 and 11.5 ${\mu}g$/mL and 88.2 and 90.5 ${\mu}M$, respectively.

Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides by Relative and Internal Monostandard Neutron Activation Analysis Methods

  • Shinde, Amol D.;Acharya, Raghunath;Reddy, Annareddy V.R.
    • Nuclear Engineering and Technology
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    • 제49권3호
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    • pp.562-568
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    • 2017
  • Background: The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Methods: Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. Results: In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. Conclusion: The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

RK-270D and E, Oxindole Derivatives from Streptomyces sp. with Anti-Angiogenic Activity

  • Jang, Jun-Pil;Jang, Mina;Nogawa, Toshihiko;Takahashi, Shunji;Osada, Hiroyuki;Ahn, Jong Seog;Ko, Sung-Kyun;Jang, Jae-Hyuk
    • Journal of Microbiology and Biotechnology
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    • 제32권3호
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    • pp.302-306
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    • 2022
  • A chemical investigation of a culture extract from Streptomyces sp. RK85-270 led to the isolation and characterization of two new oxindoles, RK-270D (1) and E (2). The structures of 1 and 2 were determined by analyzing spectroscopic and spectrometric data from 1D and 2D NMR and High-resolution electrospray ionization mass spectrometry (HRESIMS) experiments. Compound 1 exhibited anti-angiogenic activities against human umbilical vein endothelial cells (HUVECs) without cytotoxicity. Results of Western blot analysis revealed that 1 inhibits VEGF-induced angiogenesis in the HUVECs via VEGFR2/ p38 MAPK-mediated pathway.

혈액 중 PCBs 이성질체별 분석에 의한 인체 노출 평가 (Evaluation of human exposure to polychlorinated biphenyls using human serum by congener-specific analysis)

  • 박효근;이세진;김광수;강정호;백송이;장윤석
    • 분석과학
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    • 제19권1호
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    • pp.73-85
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    • 2006
  • 고분해능 가스크로마토그래피/고분해능 질량분석기를 이용하여 자원회수시설 근로자와 자원회수시설 주변 지역 주민(<0.3 km), 자원회수시설과 관련이 없는 지역주민(>10 km)의 혈액으로부터 PCBs의 모든 이성질체를 분석하였다. 전체 87개의 혈액시료 중에서 PCBs의 평균농도와 다이옥신 유사 PCBs의 평균농도는 각각 242.77 ng/g lipid, 8.83 TEQ pg/g lipid 이었다. 5, 6, 7 염소 치환 동족체가 전체 농도의 80%이상을 차지하였으며 가장 많은 농도 분포를 보이는 이성질체는 PCB153, PCB138, PCB180, PCB187, PCB118이었다. PCBs의 농도와 설문을 통해 조사된 나이, 성별, 흡연여부, 직업, BMI (Body Mass Index), 거주기간 등과 같은 변수와의 유의한 상관관계를 알기위해 통계분석을 한 결과 나이만이 혈액 내 PCBs농도와 상관관계가 있었다. 또한, 총 PCBs 농도와 PCB153 농도(r=0.93, p<.0001), dioxin-like PCBs와 PCB118의 농도(r=0.98, p<.0001)는 상관관계가 매우 높았다. 따라서 이 두 개의 이성질체는 인체 혈액에서 각각 PCBs농도와 dioxin-like PCBs의 농도의 지표물질(indicator)이 될 수 있다.

TTF 주게분자의 전구체로서 두 가지 다른 1,3-Dithiole-2-thione 화합물의 합성 및 특성화 (Synthesis and Characterization of Two Different 1,3-Dithiole-2-thiones as the Precursors of TTF Donor Molecule)

  • 김영윤;이하진;남궁성건;홍종기;노동윤
    • 대한화학회지
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    • 제44권6호
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    • pp.513-517
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    • 2000
  • TTF (tetrathiafulvalene) 유도체의 전구체로서 5,6-dimethyl-1,3-dithiolo[4,5-b][1,4]dithiin-2-thione (화합물 3)을 로손반응에 의하여 합성하였다. 치환기의 종류에 따라 1,4-dithiin이나 티오펜이 포함된 두 가지의 서로 다른 생성물이 얻어졌고, 이들은 $^{13}C$ NMR과 고 분해능 전자충돌(HREI) 질량분석 분광학으로 특성화하였다. 화합물 3의 합성은 X-선 구조분석으로도 확인되었다. 결정학적 자료: 삼사정계, 공간군 P1, a=4.145(2)${\AA}$, b=10.600(2)${\AA}$, c=12.279(2)${\AA}$, ${\alpha}=71.440(10)^{\circ},\;{\beta}=84.30(2)^{\circ},\;{\gamma}=87.31(2)^{\circ}$, Z=2, $R(wR_2$)=0.0559(0.1416). 두 가지 생성물의 생성 기구를 비교하여 설명하였다.

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Proteomic Analysis of the Aging-related Proteins in Human Normal Colon Epithelial Tissue

  • Li, Ming;Xiao, Zhi-Qiang;Chen, Zhu-Chu;Li, Jian-Ling;Li, Cui;Zhang, Peng-Fei;Li, Mao-Yu
    • BMB Reports
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    • 제40권1호
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    • pp.72-81
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    • 2007
  • In order to screen the aging related proteins in human normal colon epithelia, the comparative proteomics analysis was applied to get the two-dimensional electrophoresis (2-DE) profiles with high resolution and reproducibility from normal colon epithelial tissues of young and aged people. Differential proteins between the colon epithelia of two age groups were found with PDQuest software. The thirty five differential protein-spots were identified by peptide mass fingerprint (PMF) based on matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) and database searching. Among them there are sixteen proteins which are significantly up-regulated in the colonic mucosal epithelia of young people group, which include ATP synthase beta chain, electron transfer flavoprotein alpha-subunit, catalase, glutathione peroxidase 1, annexin A2 and heat shock cognate 71 kDa protein, etc.; There are nineteen proteins which are significantly up-regulated in the colonic mucosal epithelia of aged people group, which include far upstream element-binding protein 1, nucleoside diphosphate kinase B, protein disulfide-isomerase precursor and VDAC-2, etc.. The identified differential proteins appear to be involved in metabolism, energy generation, chaperone, antioxidation, signal transduction, protein folding and apoptosis. The data will help to understand the molecular mechanisms of human colon epithelial aging.

Comparative Proteomic Analysis of Yak Follicular Fluid during Estrus

  • Guo, Xian;Pei, Jie;Ding, Xuezhi;Chu, Min;Bao, Pengjia;Wu, Xiaoyun;Liang, Chunnian;Yan, Ping
    • Asian-Australasian Journal of Animal Sciences
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    • 제29권9호
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    • pp.1239-1246
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    • 2016
  • The breeding of yaks is highly seasonal, there are many crucial proteins involved in the reproduction control program, especially in follicular development. In order to isolate differential proteins between mature and immature follicular fluid (FF) of yak, the FF from yak follicles with different sizes were sampled respectively, and two-dimensional gel electrophoresis (2-DE) of the proteins was carried out. After silver staining, the Image Master 2D platinum software was used for protein analysis and matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF-MS) was performed for differential protein identification. The expression level of transferrin and enolase superfamily member 1 (ENOSF1) was determined by Western blotting for verification analysis. The results showed that 2-DE obtained an electrophoresis map of proteins from mature and immature yak FF with high resolution and repeatability. A comparison of protein profiles identified 12 differently expressed proteins, out of which 10 of them were upregulated while 2 were downregulated. Western blotting showed that the expression of transferrin and ENOSF1 was enhanced with follicular development. Both the obtained protein profiles and the differently expressed proteins identified in this study provided experimental data related to follicular development during yak breeding seasons. This study also laid the foundation for understanding the microenvironment during oocyte development.

Anti-Termite Activity of Azadirachta excelsa Seed Kernel and Its Isolated Compound against Coptotermes curvignathus

  • Morina ADFA;Khafit WIRADIMAFAN;Ricky Febri PRATAMA;Angga SANJAYA;Deni Agus TRIAWAN;Salprima YUDHA S.;Masayuki NINOMIYA;Mohamad RAFI;Mamoru KOKETSU
    • Journal of the Korean Wood Science and Technology
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    • 제51권3호
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    • pp.157-172
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    • 2023
  • Azadirachta excelsa, is a plant belonging to the same genus as Indian neem (Azadirachta indica), and its use as a pesticide is reported by few studies. Despite being a different species, it is expected to have the same biopesticide potential as A. indica. Therefore, this study aims to investigate the anti-termite activity of n-hexane and methanol extracts of A. excelsa seed kernel at various concentrations against Coptotermes curvignathus. The methanol extract demonstrated greater termicidal activity than n-hexane at doses test of 2%, 4%, and 8%. It also showed 100% termite mortality on the third day of administering the 8% dose. According to the gas chromatography with mass spectrometry data, the putative main components of the n-hexane extract were hexadecanoic acid, ethyl ester (18.99%), 9,12-octadecadienoic acid (Z,Z)- (16.31%), and 9-octadecenal (16.23%). In contrast, the principal constituents of methanol extract were patchouli alcohol (28.1%), delta-guaiene (15.15%), and alpha-guaiene (11.93%). Furthermore, limonoids profiling of A. excelsa methanol extract was determined using Ultrahigh-performance liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry. The number of limonoids identified tentatively was fifteen, such as 6-deacetylnimbin, nimbolidin C, nimbolide, 6-acetylnimbandiol, 6-deacetyl-nimbinene, salannol, 28-deoxonimbolide, gedunin, nimbandiol, epoxyazadiradione, azadirone, 2',3'-dihydrosalannin, marrangin, nimbocinol, and azadirachtin. They were the same as those reported in the seed and leaves of A. indica, but its largest component in A. excelsa was 6-deacetylnimbin. As a result, the presence of these compounds may be responsible for the anti-termite activity of A. excelsa seed kernel extract. Additionally, column chromatography of methanol extract yielded 6-deacetylnimbin, which was found to be antifeedant and termiticide against C. curvignathus.

하드 디스크 드라이브 회전수 변화가 드라이브 내 나노 오염 입자 발생에 미치는 영향 (Effect of Disk Rotational Speed on Contamination Nano Particles Generated in a Hard Disk Drive)

  • 이대영;황정호;배귀남
    • 대한기계학회논문집B
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    • 제28권8호
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    • pp.976-983
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    • 2004
  • In high-density hard disk drives, the slider should be made to fly close to the magnetic recording disk to generate better signal resolution and at an increasingly high velocity to achieve better data rate. The slider disk interaction in CSS (contact-start-stop) mode is an important source of particle generation. Contamination particles in the hard disk drive can cause serious problems including slider crash and thermal asperities. We investigated the number and the sizes of particles generated in the hard disk drive, operating at increasing disk rotational speeds, in the CSS mode. CNC (condensation nucleus counter) and PSS (particle size selector) were used for this investigation. In addition, we examined the particle components by using SEM (scanning electron microscopes), AES (auger electron spectroscopy), and TOF-SIMS (time of flight-secondary ions mass spectrometry). The increasing disk rotational speed directly affected the particle generation by slider disk interaction. The number of particles that were generated increased with the disk rotational speed. The particle generation rate increased rapidly at motor speeds above 8000 rpm. This increase may be due to the increased slider disk interaction. Particle sizes ranged from 14 to 200 nm. The particles generated by slider disk interaction came from the lubricant on the disk, coating layer of the disk, and also slider surface.

수입 식육의 안전성 확보를 위한 polychlorinated dibenzo-p-dioxins와 dibenzofurans 분석 (Analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans to assure safety of imported meat)

  • 김미경;김동규;김수연;최시원;권진욱;윤선종;송성옥;정갑수
    • 대한수의학회지
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    • 제48권1호
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    • pp.39-48
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    • 2008
  • Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) are ubiquitous and can contaminate the food chain. A study monitoring PCDD/Fs in imported meat was conducted at the National Veterinary Research and Quarantine Service (NVRQS, Republic of Korea) in order to maintain food safety from the bioaccumulative PCDD/Fs. Seventeen PCDD/Fs with toxic equivalency factors (TEFs) established by World Health Organization (WHO, 1998) were analyzed in imported beef, pork, and chicken by high resolution gas chromatography/mass spectrometry (HR-GC/MS). Results of the monitoring for the last 5 years are presented. The levels of PCDD/Fs were similar to other studies except two unusually high concentrations in pork and beef. Excessive levels greater than the Korean provisional maximum residue limit of PCDD/Fs were found in a sample of pork imported from Chile and a sample of beef imported from U.S, and those products were rejected and returned. There was no obvious trend or differences with respect to time or origin of meat in this study.