• Title/Summary/Keyword: 2-D LC MS/MS

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α-Glucosidase inhibitory caged xanthones from the resin of Garcinia hanburyi

  • Jin, Young Min;Kim, Jeong Yoon;Lee, Soo Min;Tan, Xue Fei;Park, Ki Hun
    • Journal of Applied Biological Chemistry
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    • v.62 no.1
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    • pp.81-86
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    • 2019
  • A yellow resin (gamboge) from Garcinia hanburyi has been widely used as folk medicine due to its antibacterial and antitumor activities. We isolated four ${\alpha}$-glucosidase inhibitory compounds from the methanol extract of gamboge. The compounds (1-4) were identified as gambogoic acid (1), moreollic acid (2), gambogic acid (3), and 10-methoxygambogenic acid (4), respectively through spectroscopic data including 2D-NMR and HREIMS. All compounds were examined in the enzyme inhibition assay against ${\alpha}$-glucosidase to identify their inhibitory potencies and kinetic behavior. All compounds (1-4) showed enzyme inhibition against ${\alpha}$-glucosidase, but the activity was significantly affected by the methoxy group on C-10 of ring A and pentenyl pyran moiety of ring D. For example, compound 1 ($IC_{50}=41.4{\mu}M$) bearing pyran ring eight times effective that 4 ($IC_{50}=350.6{\mu}M$) having geranyl group itself. Most active compound was found out to be gambogoic acid (1) which was analyzed most abundant metabolite in gamboge by LC-ESI-MS/MS. In kinetic study, compounds 1 and 2 were proved as noncompetitive inhibitors.

Qualitative and Quantitative Analysis of Thirteen Marker Components in Traditional Korean Formula, Samryeongbaekchul-san using an Ultra-Performance Liquid Chromatography Equipped with Electrospray Ionization Tandem Mass Spectrometry

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.22 no.2
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    • pp.93-101
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    • 2016
  • For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ${\geq}0.9920$ within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and $115.01{\mu}g/g$, respectively.

Research on the Possibility of Using Wrinkle-improving Functional Materials from Corn By-products (옥수수 부산물을 이용한 주름 개선 기능성 소재 활용 가능성 연구)

  • Hye Jin Kim;Woo Seok Choi;June Seob Lee;Ja Young Kim;Moo-Han Kim;Chang Hyeon Lee
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.49 no.2
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    • pp.107-116
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    • 2023
  • In this study, to explore the possibility of using discarded by-products of corn as a wrinkle-improving functional material, the active ingredient contained in each part including kernel, cob, husk, and silk of 10 varieties of chodang and waxy corn was identified and the content was analyzed to suggest the possibility of corn by-products as upcycling materials. As a result of evaluating the collagen synthesis efficacy of extracts by part, the cob in chodang and waxy corns showed significant activity at 100 ㎍/mL concentration of 176.5 and 140.0%, respectively. The LC-MS/MS qualitative analysis resulted in the identification of 18 components in the cob, of which N, N'-diferuloylputrescine (DFP) was selected as an active ingredient, and the quantitative analysis was conducted by variety and part. As a result, DFP was confirmed only in the cob and kernel, and it was most frequently detected in the cob of the Goldsugar of chodang corn (39.6 ㎍/g) and Daehakchal of waxy corn (38.4 ㎍/g). The cob is a by-product left over from grain removal, and is expected to create new added value as a material that promotes collagen synthesis. Through this study, we propose the possibility of using discarded cob as a wrinkle-improving functional material.

Bioequivalence of Efexor® XR capsule to Venfaxine® OR tablet (Venlafaxine 75 mg) (이팩사® XR서방캅셀(벤라팍신, 75 mg)에 대한 벤팍신®OR서방정의 생물학적동등성)

  • Aryal, Dipendra Kumar;Oh, Soo-Yeon;Cho, Jong-Tae;Kim, Hyung-Gun;Kim, Yoon-Gyoon
    • Journal of Pharmaceutical Investigation
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    • v.37 no.6
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    • pp.397-402
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    • 2007
  • To evaluate the bioequivalence of two venlafaxine formulations, a standard 2-way randomized cross-over study was conducted in twenty-four healthy male Korean volunteers. A single oral dose of 75 mg of test formulation Venfaxine $OR^{(R)}$ (tablet) or reference formulation Efexor $XR^{(R)}$ (capsule) was administered with one-week washout period. Plasma concentrations of venlafaxine were assayed for over a period of 72 hours with a well validated method using liquid chromatography coupled to tandem mass spectrometry (LC-MS-MS). The $mean{\pm}S.D$. of maximum concentration $(C_{max})$ and elimination half-life $(t_{1/2})$ were $64.7{\pm}28.5$ ng/mL, $9.2{\pm}3.0$ h, and $67.2{\pm}30.2$ ng/mL, $9.9{\pm}3.5$ h for test and reference formulations, respectively. Time to reach maximum concentration $(T_{max})$ expressed in median value (range), for the test and the reference, were 10 h (6-14) and 8h (4-12), respectively. Similarly, area under the plasma concentration-time curve, from time zero to last sampling time $(AUC_t)$ and from time zero to time infinity $(AUC_{inf})$, for test and reference formulations were $1185{\pm}755$, $1326{\pm}896$ and $1124{\pm}737$, $1185{\pm}755$ $ng{\cdot}h/mL$, respectively. The parametric 90% confidence intervals on the mean of the differences between the two formulations (test-reference) of the log transformed values of $AUC_t$, and $C_{max}$ were 0.9630 to 1.1383 and 0.8650 to 1.0446, respectively. The overall results indicate that the two formulations are bioequivalent and can be prescribe interchangeably.

Biosynthesis of Bile Acids in a Variety of Marine Bacterial Taxa

  • Kim, Doc-Kyu;Lee, Jong-Suk;Kim, Ji-Young;Kang, So-Jung;Yoon, Jung-Hoon;Kim, Won-Gon;Lee, Choong-Hwan
    • Journal of Microbiology and Biotechnology
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    • v.17 no.3
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    • pp.403-407
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    • 2007
  • Several marine. bacterial strains, which were isolated from seawater off the island Dokdo, Korea, were screened to find new bioactive compounds such as antibiotics. Among them, Donghaeana dokdonensis strain DSW-6 was found to produce antibacterial agents, and the agents were then purified and analyzed by LC-MS/MS and 1D- and 2D-NMR spectrometries. The bioactive compounds were successfully identified as cholic acid and glycine-conjugated glycocholic acid, the $7{\alpha}$-dehydroxylated derivatives (deoxycholic acid and glycodeoxycholic acid) of which were also detected in relatively small amounts. Other marine isolates, taxonomically different from DSW-6, were also able to produce the compounds in a quite different production ratio from DSW-6. As far as we are aware of, these bile acids are produced by specific members of the genus Streptomyces and Myroides, and thought to be general secondary metabolites produced by a variety of bacterial taxa that are widely distributed in the sea.

Anti-inflammatory Action of Herbal Medicine Comprised of Scutellaria baicalensis and Chrysanthemum morifolium

  • Min Geun Suh;Hyeon-Son Choi;Kyoungwon Cho;Sung Sun Park;Woo Jung Kim;Hyung Joo Suh;Hoon Kim
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2020.08a
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    • pp.72-72
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    • 2020
  • Various mixtures were prepared depending on the mixing ratio of Scutellaria baicalensis hot water extract (SB-HW) and Chrysanthemum morifolium ethanol extract (CM-E) and their anti-inflammatory activity were compared. Among them, SB-HW (80 ㎍/mL)/CM-E (120 ㎍/mL) or SB-HW (40 ㎍/mL)/CM-E (160 ㎍/mL) significantly inhibited LPS-stimulated NO and IL-6 levels in RAW 264.7 cells. The SB-HW (80 ㎍/mL)/CM-E (120 ㎍/mL) mixture, which was determined as active mixture, significantly reduced MUC5AC secretion in PMA and LPS-induced NCI-H292 cells. The active mixture also reduced the production of PGE2 and IL-8 in PMA-induced A549 cells. LC-MS/MS analysis showed that the active mixture was composed of high contents of flavone glycosides, such as baicalin and cynaroside. Western blot analysis indicated that the active mixture suppressed phosphorylation of ERK, JNK, and p38, associating with the inhibition of MAPK signaling. Taken together, our results suggest that the active mixture could be applied as a new anti-inflammatory herbal medicine

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Flavonoids from the Stems of Eastern Picklypear Opuntia humifusa, Cactaceae

  • Park, Si-Hyung;Kim, Hui;Rhyu, Dong-Young
    • Journal of Applied Biological Chemistry
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    • v.50 no.4
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    • pp.254-258
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    • 2007
  • Five flavonoids, isorhamnetin 3-O-${\beta}$-D-galactosyl-4'-O-${\beta}$-D-glucoside (1), isorhamnetin 3,4'-di-O-${\beta}$-D-glucoside (2), isorhamnetin 3-O-${\beta}$-D-(6-O-${\alpha}$-L-rhamnosyl)glucosyl-4'-O-${\beta}$-D-glucoside (3), isorhamnetin 3-O-${\beta}$-D-(6-O-${\alpha}$-L-rhamnosyl)glucoside (4), and isorhamnetin 3-O-${\beta}$-D-(6-O-${\alpha}$-L-rhamnosyl) galactoside (5) were isolated from the stems of Opuntia humifusa (Raf.) Raf. and their structures were identified based on LC-MS and NMR data.

Synthesis and radiolabeling of PEGylated dendrimer-G2-Gemifloxacin with 99mTc to Biodistribution study in rabbit

  • Mohtavinejad, Naser;Dolatshahi, Shaya;Amanlou, Massoud;Ardestani, Mehdi Shafiee;Asadi, Mehdi;Pormohammad, Ali
    • Advances in nano research
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    • v.10 no.5
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    • pp.461-470
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    • 2021
  • Infection is one of the major mortality causes throughout the globe. Nuclear medicine plays an important role in diagnosis of deep infections such as osteomyelitis, arthritis infection, heart valve and heart prosthesis infections. Techniques such as labeled leukocytes are sensitive and selective for tracking the inflammations but they are not suitable for differentiating infection from inflammation. Anionic linear-globular dendrimer-G2 was synthesized then conjugation to gemifloxacin antibiotic. The structures were identified by FT-IR, 1H-NMR, C-NMR, LC-MS and DLS. The toxicity of gemifloxacin and dendrimer-gemifloxacin complex was compared by MTT test. Dendrimer-G2-gemifloxacin was labeled by Technetium-99m and its in-vitro stability and radiochemical purity were investigated. In-vivo biodistribution and SPECT imaging were studied in a rabbit model. Identify and verify the structure of the each object was confirmed by FT-IR, 1H-NMR, C-NMR and LC-MS, also, the size and charge of this compound were 128 nm and -3/68 mv respectively. MTT test showed less toxicity of the dendrimer-G2-gemifloxacin than free gemifluxacin (P < 0.001). Radiochemical yield was > %98. Human serum stability was 84% up to 24 h. Biodistribution study at 50 min, 24 and 48 h showed that the complex is significantly absorbed by the intestine and accumulation in the lungs and affects them, finally excreted through the kidneys, biodistribution results are consistent with results from full image means of SPECT/CT technique.

The Physiological Role of CPR1 in Saccharomyces cerevisiae KNU5377 against Menadione Stress by Proteomics

  • Kim, Il-Sup;Yun, Hae-Sun;Kwak, Sun-Hye;Jin, Ing-Nyol
    • Journal of Microbiology
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    • v.45 no.4
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    • pp.326-332
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    • 2007
  • In order to understand the functional role of CPRl in Saccharomyces cerevisiae KNU5377 with regard to its multi-tolerance characteristics against high temperatures, inorganic acids, and oxidative stress conditions, whole cellular proteins were analyzed via liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). This procedure was followed by two-dimensional (2-D) gel electrophoresis. Under menadione stress conditions, the 23 upregulated proteins were clearly identified only in the wild- type strain of KNU5377. Among the proteins, Sodl1p Tsa1p, Ahp1, Cpr1p, Cpr3, Ssb2p, and Hsp12p were identified as components of antioxidant systems or protein-folding related systems. The CPR1 protein could not be completely detected in the $cpr1{\Delta}$ mutant of KNU5377 and the other upregulated proteins in the wild-type strain evidenced a clear correlation with the results of immunoblot analysis. Moreover, a reduction in growth patterns (about 50%) could be observed in the $cpr1{\Delta}$ mutant, as compared with that of the wild-type strain under mild MD stress conditions. These results indicate that the upregulation of CPR1 may contribute to tolerance against MD as an inducer of oxidative stress.

Proteomics Analysis of Early Salt-Responsive Proteins in Ginseng (Panax ginseng C. A. Meyer) Leaves (초기 염류 스트레스 반응 인삼 잎 단백질체 분석)

  • Kim, So Wun;Min, Chul Woo;Gupta, Ravi;Jo, Ick Hyun;Bang, Kyong Hwan;Kim, Young-Chang;Kim, Kee-Hong;Kim, Sun Tae
    • Korean Journal of Medicinal Crop Science
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    • v.22 no.5
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    • pp.398-404
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    • 2014
  • Salt stress is one of the major abiotic stresses affecting the yield of ginseng (Panax ginseng C. A. Meyer). The objective of this study was to identify bio-marker, which is early responsive in salt stress in ginseng, using proteomics approach. Ginseng plants were exposed to 5 ds/m salt concentration and samples were harvested at 0, 6, 12 and 18 hours after exposure. Total proteins were extracted from ginseng leaves treated with salt stress using Mg/NP-40 buffer and were separated on high resolution 2-DE. Approximately $1003{\pm}240$ (0 h), $992{\pm}166$ (6 h), $1051{\pm}51$ (12 h) and $990{\pm}160$ (18 h) spots were detected in colloidal CBB stained 2D maps. Among these, 8 spots were differentially expressed and were identified by using MALDI-TOF/TOF MS or/and LC-MS/MS. Ethylene response sensor-1 (spot GL 1), nucleotide binding protein (spot GL 2), carbonic anhydrase-1 (spot GL 3), thylakoid lumenal 17.9 kDa protein (spot GL 4) and Chlorophyll a/b binding protein (spot GL 5, GL 6) were up-regulated at the 12 and 18 hour, while RuBisCO activase B (spot GL 7) and DNA helicase (spot GL 8) were down-regulated. Thus, we suggest that these proteins might participate in the early response to salt stress in ginseng leaves.