• Title/Summary/Keyword: high performance liquid chromatography-mass spectrometry (HPLC-MS)

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Tyrosinase Inhibitory Compounds Isolated from Persicaria tinctoria Flower (쪽 꽃에서 분리한 타이로시네이즈 저해 화합물)

  • Woo, Young-Min;Kim, Ah-Jin;Kim, Ji-Young;Lee, Choong-Hwan
    • Journal of Applied Biological Chemistry
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    • v.54 no.1
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    • pp.47-50
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    • 2011
  • To develop a new natural whitening agent, we investigated the tyrosinase inhibitory effects of Persicaria tinctoria Flower extracts (PTFE). PTFE showed inhibitory activity on mushroom tyrosinase with the $IC_{50}$ values of $70.8{\pm}2.2{\mu}g/mL$. We purified two active compounds from PTFE by LH-20 column chromatography and prep-high performance liquid chromatography (HPLC) and identified as quercetin-3-O-rhamnoside (Q3R) and myricetin-3-O-rhamnoside (M3R) by $^1H$nuclear magnetic resonance (NMR) and liquid chromatography-mass spectrometry (LC-MS) analysis. Q3R and M3R showed tyrosinase inhibitory activities with the $IC_{50}$ values of $47.0{\pm}0.1{\mu}g/mL$ and $150.5{\pm}1.6{\mu}g/mL$, respectively. These results suggest that PTFE and its active compounds reduced melanin formation by the inhibition of tyrosinase activity. Thus, P. tinctoria flower extracts may be a candidate for cosmetic use.

Enzymatic Synthesis and Characterization of Galactosyl Trehalose Trisaccharides

  • Kim, Bong-Gwan;Lee, Kyung-Ju;Han, Nam-Soo;Park, Kwan-Hwa;Lee, Soo-Bok
    • Food Science and Biotechnology
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    • v.16 no.1
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    • pp.127-132
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    • 2007
  • [ ${\alpha},\;{\alpha}$ ]-Trehalose was efficiently modified by a transgalactosylation reaction of Escherichia coli ${\beta}-galactosidase$ using lactose as a donor to yield two galactosyl trehalose trisaccharides. The reaction products of trehalose by the enzyme were observed by thin layer chromatography (TLC) and high performance anion exchange chromatography (HPAEC) and were purified by BioGel P2 gel permeation chromatography and recycling preparative HPLC. Liquid chromatography-mass spectrometry (LC-MS) and ^{13}C$ nuclear magnetic resonance (NMR) analyses revealed that the structures of the main products were $6^2-{\beta}-D-galactosyl$ trehalose (1) and $4^2-{\beta}-D-galactosyl$ trehalose (2). A reaction of 30%(w/v) trehalose and 15%(w/v) lactose at pH 7.5 and $45^{\circ}C$ resulted in a total yield of approximately 27-30% based on the amount of trehalose used. The galactosyl trehalose products were not hydrolyzed by trehalose. In addition the mixture of transfer products (9:1 ratio of 1 to 2) showed higher thermal stability than glucose, lactose, and maltose, but less than trehalose, against heat treatment over $100^{\circ}C$ at pH 4 and 7. It also exhibited better thermal stability than sucrose at pH 4 alone.

Antibacterial compounds against fish pathogenic bacteria from a combined extract of Angelica gigas and Artemisia iwayomogi and their quantitative analyses

  • Lim, Jae-Woong;Kim, Na Young;Seo, Jung-Soo;Jung, Sung-Hee;Kang, So Young
    • Fisheries and Aquatic Sciences
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    • v.24 no.10
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    • pp.319-329
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    • 2021
  • In the search for antibiotic alternatives from safe and effective medicinal plants against fish pathogenic bacteria, we found that a combined extract (CE) of 1:1 (w/w) ratio of Angelica gigas Nakai roots and aerial parts of Artemisia iwayomogi Kitamura showed antibacterial activity against the fish pathogenic bacteria. By antibacterial activity-guided fractionations and isolations, five compounds were isolated and identified as decursinol angelate (1), decursin (2), xanthotoxin (3), demethylsuberosin (4), and 2,4-dihydroxy-6-methoxyacetophenone (5) through spectroscopic analyses, such as nuclear magnetic resonance (NMR) and mass spectrometry (MS). Among the compounds, 1 and 2 showed the highest antibacterial activities against Streptococcus iniae and Vibrio anguillarum, showing minimum inhibitory concentrations (MICs) of 62.5-250 ㎍/mL. Compounds 3, 4, and 5 were also found to be active, with MICs of 31.25-1,000 ㎍/mL for those strains. Furthermore, active compounds, 1 and 2 in CE were simultaneously quantified using high-performance liquid chromatography-tandem MS (HPLC-MS/MS). The average contents of 1 and 2 in CE was 3.68% and 6.14%, respectively. The established method showed reliable linearity (r2 > 0.99), good precision, accuracy, and specificity with intra- and inter-day variations of < 2 % and recoveries of 90.13%-108.57%. These results may be helpful for establishing the chemical profile of CE for its commercialization as an antibiotic alternative in aquaculture.

Antibacterial and Antibiofilm Activities of Diospyros malabarica Stem Extract against Streptococcus mutans (Streptococcus mutans에 대한 인도감나무 줄기 추출물의 항균활성 및 생물막 형성 억제 효과)

  • Kim, Hye Soo;Lee, Sang Woo;Sydara, Kongmany;Cho, Soo Jeong
    • Journal of Life Science
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    • v.29 no.1
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    • pp.90-96
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    • 2019
  • The objective of this study was to evaluate the potential of Diospyros malabarica stem extract, a natural materials, in oral health material. With this aim in mind, thin layer chromatography (TLC), TLC-bioautography, high-performance liquid chromatography (HPLC), electrospray ionization-mass spectrometry (ESI-MS), scanning electron microscopy (SEM), and real-time qPCR were performed. The antibacterial activity of D. malabarica stem extract against Streptococcus mutans KCTC3065 was confirmed in an n-hexane fraction with low polarity. The molecular weight of the antibacterial compound was estimated to be 188 by ESI-MS analysis. The inhibitory effects of the extract on biofilm formation and gene expression related to biofilm formation of S. mutans were determined by SEM and real-time PCR analysis. The extract inhibited the formation of S. mutans biofilms at D. malabarica stem extract concentrations of 1 mg/ml, as shown by SEM. The real-time PCR analysis showed that the expression of the gtfC gene, which is associated with biofilm formation, was significantly decreased in a dose-dependent manner. Based on the above results, it can be concluded that D. malabarica stem extracts, a natural materials, can be used in oral health products to suppress the formation of biofilms by inhibiting tooth adhesion of S. mutans, a causative agent of dental caries.

Cardioprotective effect of ginsenoside Rb1 via regulating metabolomics profiling and AMP-activated protein kinase-dependent mitophagy

  • Hu, Jingui;Zhang, Ling;Fu, Fei;Lai, Qiong;Zhang, Lu;Liu, Tao;Yu, Boyang;Kou, Junping;Li, Fang
    • Journal of Ginseng Research
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    • v.46 no.2
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    • pp.255-265
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    • 2022
  • Background: Ginsenoside Rb1, a bioactive component isolated from the Panax ginseng, acts as a remedy to prevent myocardial injury. However, it is obscure whether the cardioprotective functions of Rb1 are related to the regulation of endogenous metabolites, and its potential molecular mechanism still needs further clarification, especially from a comprehensive metabolomics profiling perspective. Methods: The mice model of acute myocardial ischemia (AMI) and oxygen glucose deprivation (OGD)-induced cardiomyocytes injury were applied to explore the protective effect and mechanism of Rb1. Meanwhile, the comprehensive metabolomics profiling was conducted by high-performance liquid chromatography and quadrupole time-of-flight mass spectrometry (HPLC-Q/TOF-MS) and a tandem liquid chromatography and mass spectrometry (LC-MS). Results: Rb1 treatment profoundly reduced the infarct size and attenuated myocardial injury. The metabolic network map of 65 differential endogenous metabolites was constructed and provided a new inspiration for the treatment of AMI by Rb1, which was mainly associated with mitophagy. In vivo and in vitro experiments, Rb1 was found to improve mitochondrial morphology, mitochondrial function and promote mitophagy. Interestingly, the mitophagy inhibitor partly attenuated the cardioprotective effect of Rb1. Additionally, Rb1 markedly facilitated the phosphorylation of AMP-activated protein kinase α (AMPKα), and AMPK inhibition partially weakened the role of Rb1 in promoting mitophagy. Conclusions: Ginsenoside Rb1 protects acute myocardial ischemia injury through promoting mitophagy via AMPKα phosphorylation, which might lay the foundation for the further application of Rb1 in cardiovascular diseases.

Component Analysis of Suaeda asparagoides Extracts (나문재 추출물의 성분 분석)

  • Yang, Hee-Jung;Park, Soo-Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.3
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    • pp.157-165
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    • 2008
  • In the previous study, the anti-oxidant activity of oxtract/fraction of Sueada aspparagoides(SA) and the stability test for the cream containing SA extract were investigated respectively[1,2]. In this study, the components of SA extract were analyzed by TLC, HPLC, and LC/ESI-MS/MS, $^1H$-NMR. TLC chromatogram of ethyl acetate fraction of SA extract revealed 5 bands $(SA1{\sim}SA5)$. HPLC chromatogram of aglycone fractions obtained from deglycoylation reaction of ethyl acetate fraction showed 2 bands (SAA 2 and SAA 1), which were identified as quercetin (composition ratio, 16.88%) and kaempferol (83.12%) in the order of elution time. Among 5 bands of TLC chromatogram, 4 bands $(SA2{\sim}SA5)$ also were Identified as kaempferol-3-O-glucoside (SA 2), quercetin-3-O-glucoside (SA3), kaempferol-3-O-rutinoside (SA 4), quercetin-3-O-rutinoside (SA 5) by LC/ESI-MS/MSMS/MS. respectively. The spectrum generated for SAA 1 by LC/ESI-MS/MS in the negative ion mode also gave the ion corresponding to the deprotonated aglycone $[M-H]^-$ (285m/z), the $^1H$-NMR spectrum contained signals [${\delta}$ 6.19 (1H, d, J=1.8Hz, H-6), ${\delta}$ 6.44 (1H, d, J=1.8Hz, H-8), ${\delta}$ 6.92 (2H, d, J=9.0Hz, H-3', 5'), ${\delta}$ 8.04 (2H, d, J=9.0Hz, H-2', 6', thus SAA 1 was identified as kaempferol. SAA 2 yielded the deprotonated agycone ion $[M-H]^-$ (301m/z), $^1H$-NMR spectrum showed signals [${\delta}$ 6.20 (1H, d, J=2.0Hz, H-6), ${\delta}$ 6.42 (1H, d, J=2.0Hz, H-8), ${\delta}$ 6.90 (1H, d, J=8.6Hz, H-5'), ${\delta}$ 7.55 (1H, dd, J=8.6, 2.2Hz, H-6'), ${\delta}$ 7.69 (1H, d, J=2.2Hz, H-2', thus SAA 2 was Identified as quercetin. In conclusion, with the anti-oxidant activity and the stability test reported previously, component analysis of SA extracts could be applicable to new cosmeceuticals.

Monitoring of Benzoic, Sorbic and Propionic Acid in Cereal Grains, Nuts and Seeds (곡류 및 견과 종실류 중 안식향산, 소브산, 프로피온산의 함유량 조사)

  • Yun, Sang Soon;Lee, Sang Jin;Lim, Do Yeon;Lim, Ho Soo;Lee, Gunyoung;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.65-72
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    • 2019
  • This study was aimed at investigating the levels of the natural preservatives of benzoic, sorbic and propionic acids in cereal grains, nuts and seeds. Benzoic and sorbic acid were analyzed by high-performance liquid chromatography with a diode-array detector (HPLC-DAD) and further confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), whereas propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and further confirmed by gas chromatography-mass spectrometry (GC-MS). Benzoic, sorbic and propionic acids were found in 44, 22, and 550 samples out of 702 samples, respectively. From the total of 702 samples. The concentrations of benzoic, sorbic and propionic acid were ranged from not detected (ND) to 23.74 mg/L, from ND to 7.90 mg/L, and from ND to 37.39 mg/L in cereal grains, nuts and seeds, respectively. The concentration ranges determined in this study could be used as standard criteria in the process of inspecting cereal grains, nuts and seeds for preservatives as well as to address consumer complaints or trade disputes.

Isolation and Identification of Two Flavonoids from Pear (Pyrus pyrifolia Nakai cv. Chuhwangbae) Fruit Peel (추황배(Pyrus pyrifolia Nakai cv. Chuhwangbae) 과피로부터 2종의 Flavonoids의 단리·동정)

  • Lee, Sang Won;Lee, Yu Geon;Cho, Jeong-Yong;Kim, Young Chool;Lee, Sang-Hyun;Kim, Wol-Soo;Moon, Jae-Hak
    • Korean Journal of Food Science and Technology
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    • v.47 no.2
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    • pp.170-175
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    • 2015
  • The methanol extract of Asian pear (Pyrus pyrifolia N. cv. Chuhwangbae) fruit peel was purified using solvent fractionation, Sephadex LH-20 column chromatography, and octadecylsilane high performance liquid chromatography. Based on the electrospray ionization mass spectrometry and nuclear magnetic resonance data, the two isolated compounds were identified as quercetin 3-O-${\beta}$-D-glucopyranoside (1) and 3,5,6,7,8,3',4'-heptahydroxyflavan [(-)-dulcisflavan, 2]. Compounds 1 and 2 were isolated and identified for the first time from Asian pears and pears, respectively.

Determination of fuel marker in petroleum products using GC-MS (GC-MS를 이용한 석유제품 중의 식별제 분석)

  • Youn, Ju Min;Doe, Jin Woo;Yim, Eui Soon;Lee, Jung Min
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.1073-1080
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    • 2018
  • There are several types of petroleum products used for the fuel oil, according to their respective quality standards, grades and usage. Depending on the degree of oil tax rate by country, even the same petroleum products will have price gap. The illegal mixing of cheap petroleum products, which are subject to the lower tax rate, with relatively expensive transportation fuel causes problems such as tax evasion, environmental pollution and vehicle breakdown. In order to prevent illicit production and mixing of these different petroleum products, a small amount of markers are legally added to specific petroleum products. In Korea, markers are introduced and used to prevent illegal activity that kerosene used as fuel for house and commercial boiler are mixed with automotive diesel fuels, and marker contents are analyzed to use UV-Vis spectrophotometer and high performance liquid chromatography (HPLC). In this study, we have developed a method to qualitatively and quantitatively determine the marker added to petroleum products by gas chromatography-mass spectrometry (GC-MS) without adding developing reagent or sample pre-treatments.

First record of a marine microalgal species, Micractinium singularis (Trebouxiophyceae) isolated from Janghang Harbor, Korea

  • Jo, Seung-Woo;Kang, Nam Seon;Chae, Hyunsik;Lee, Jung A;Kim, Kyeong Mi;Yoon, Moongeun;Hong, Ji Won;Yoon, Ho-Sung
    • Korean Journal of Environmental Biology
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    • v.38 no.1
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    • pp.61-70
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    • 2020
  • A eukaryotic microalga was isolated from seawater in Janghang Harbor, Korea and its morphological, molecular, and physiological characteristics were investigated. Due to its simple morphology, no distinctive characters were found by morphological observation, such as light microscope or scanning/transmission electron microscopy (S/TEM). However, molecular phylogenetic evidence inferred from the concatenated small subunit (SSU) 18S rRNA and internal transcribed spacer (ITS) sequence data indicated that the isolate belonged to the newly described Micractinium singularis. Furthermore, it was clustered with Antarctic Micractinium strains and it also showed a psychrotolerant property, surviving at temperatures as low as 5℃. However, its optimal growth temperatures range from 15℃ to 25℃, indicating that this microalga is a mesophile. Additionally, gas chromatography-mass spectrometry (GC/MS) analysis showed that the isolate was rich in nutritionally important omega-3 polyunsaturated fatty acid, and high-performance liquid chromatography analysis (HPLC) revealed that the high-value antioxidant lutein was biosynthesized as an accessory pigment by this microalga, with glucose as the major monosaccharide. Therefore, in this study, a Korean marine M. singularis species was discovered, characterized, and described. It was subsequently added to the national culture collections.