• Title/Summary/Keyword: UPLC/MS/MS

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Purification and Characterization of Antibacterial Compound Produced by Bacillus subtilis MJP1 (Bacillus subtilis MJP1이 생산하는 항세균 물질의 분리.정제 및 특성규명)

  • Yim, Eun-Jung;Yang, Eun-Ju;Chang, Hae-Choon
    • Microbiology and Biotechnology Letters
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    • v.38 no.1
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    • pp.84-92
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    • 2010
  • Antibacterial compound from Bacillus subtilis MJP1 was purified using C18 Sep-Pak cartridge, ion exchange chromatography, and gel filtration chromatography. The purified antibacterial compound showed antibacterial activity against Listeria monocytogenes, Bacillus subtilis, Staphylococcus aureus subsp. aureus, and Enterococcus faecalis. The purified antibacterial compound was found to be stable at $100^{\circ}C$ for 5 min and in the pH range of 3.0~9.0, but it was unstable at pH 10.0. It was inactivated by proteinase K and pronase E, and heat treatment at $121^{\circ}C$ for 15 min, but it was stable with lipase and $\alpha$-amylase treatment, which indicated its proteineous nature. Ultra performance liquid chromatography and electrospray ionization tandem mass spectrometry analysis were used to identify the purified antibacterial compound and confirmed the existence of two peptides (3356.54 Da, 3400.5244 Da).

Chemical transformation and target preparation of saponins in stems and leaves of Panax notoginseng

  • Wang, Ru-Feng;Li, Juan;Hu, Hai-Jun;Li, Jia;Yang, Ying-Bo;Yang, Li;Wang, Zheng-Tao
    • Journal of Ginseng Research
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    • v.42 no.3
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    • pp.270-276
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    • 2018
  • Background: Notoginsenoside Ft1 is a promising potential candidate for cardiovascular and cancer disease therapy owing to its positive pharmacological activities. However, the yield of Ft1 is ultralow utilizing reported methods. Herein, an acid hydrolyzing strategy was implemented in the acquirement of rare notoginsenoside Ft1. Methods: Chemical profiles were identified by ultraperformance liquid chromatography coupled with quadruple-time-of-flight and electrospray ionization mass spectrometry (UPLC-Q/TOF-ESI-MS). The acid hydrolyzing dynamic changes of chemical compositions and the possible transformation pathways of saponins were monitored by ultrahigh-performance LC coupled with tandem MS (UHPLC-MS/ MS). Results and conclusion: Notoginsenoside Ft1 was epimerized from notoginsenoside ST4, which was generated through cleaving the carbohydrate side chains at C-20 of notoginsenosides Fa and Fc, and vinaginsenoside R7, and further converted to other compounds via hydroxylation at C-25 or hydrolysis of the carbohydrate side chains at C-3 under the acid conditions. High temperature contributed to the hydroxylation reaction at C-25 and 25% acetic acid concentration was conducive to the preparation of notoginsenoside Ft1. C-20 epimers of notoginsenoside Ft1 and ST4 were successfully separated utilizing solvent method of acetic acid solution. The theoretical preparation yield rate of notoginsenoside Ft1 was about 1.8%, which would be beneficial to further study on its bioactivities and clinical application.

Isolation and Identification of Anthocyanins and Determination of Antioxidative Activity in Rice-hull of a new Cultivar, 'Jungmo1020' ('중모1020' 왕겨의 안토시아닌 동정 및 항산화 효과 검정)

  • Ra, Ji-Eun;Park, Ji-Young;Seo, Woo Duck;Song, You-Chun;Cho, Jun-Hyun;Lee, Jong-Hee;Sim, Eun-Yeong;Nam, Min-Hee;Chung, Ill-Min;Han, Sang-Ik
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.59 no.4
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    • pp.391-397
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    • 2014
  • Anthocyanins are water-soluble plant pigments that give rise to the red, purple, or blue colors observed in many crops. Especially purple pigment of colored rice represent biological activities has been an increased interest, due to the functional meal as a staple food. These health benefits have been attributed to antioxidant property of anthocyanin. However, there have been little genetic source for development of new and various colored rice variety. A recently developed new variety, 'Jungmo1020', showed an unique characteristic of blue color of rice grain hull. We identified the pigment petunidin-3-O-glucoside (Pt-3-G) as a major compound with a value of $176.3{\pm}2.3mg/100g$ (68.3%) from 80% MeOH with 1% HCl extracts by UPLC/MS/MS. The content of Pt-3-G in the extracts using a solvent of 100% MeOH with 1% HCl was the highest with the values of $183.8{\pm}2.5mg/100g$. In addition, these extracts showed excellent antioxidatative activities by DPPH and ABTs assay.

Synthesis and Structural Characterization of β-Carboline Compounds (β-카볼린 화합물의 합성 및 구조분석)

  • Byeon, Hong-Ju;Han, Min-Hui;Moon, Gi-Seong;Jung, Kyung-Hwan;Lee, Hyang-Yeol
    • Journal of the Korean Applied Science and Technology
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    • v.36 no.2
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    • pp.676-684
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    • 2019
  • The Pictet-Spengler reactions have widely known for the organic synthesis or biosynthesis of biologically active compounds, tetrahydro-${\beta}$-carbolines. We have developed the simple and efficient synthetic method for the synthesis of ${\beta}$-carbolines in water. Their chemical structures were characterized by nmr and UPLC/MS/QTOF. Calculated masses of compound 1 ($C_{17}H_{17}N_2$ 249.1392), 2 ($C_{17}H_{23}N_2$ 255.1861), 3 ($C_{19}H_{21}N_2O_3$ 325.1552) and 4 ($C_{19}H_{19}N_2O$ 279.1497) were almost identical with the detected masses of compound 1 (249.1315), 2 (255.1789), 3 (325.1460) and 4 (279.1364) respectively. Those synthesized four compounds showed strong antibiotic activity against the common E. coli.

Characterization of Isoflavones from Seed of Selected Soybean (Glycine max L.) Resources Using High-Resolution Mass Spectrometry (고해상도 질량 분석을 이용한 대두(Glycine max L.) 우수자원 종자의 이소플라본 특성 평가)

  • Lee, So-Jeong;Kim, Heon-Woong;Lee, Suji;Na, Hyemin;Kwon, Ryeong Ha;Kim, Ju Hyung;Yoon, Hyemyeong;Choi, Yu-Mi;Wee, Chi-Do;Yoo, Seon Mi;Lee, Sang Hoon
    • The Korean Journal of Food And Nutrition
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    • v.33 no.6
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    • pp.655-665
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    • 2020
  • In this study, chemical information on a total of 20 individual compounds was constructed to identify isoflavones from the previous reports related with used parts(seeds, leaves, stems, pods) and products of soybean(Glycine max L.). Through constructed library and UPLC-DAD-QToF/MS analysis, a total of 19 individual isoflavones including aglycones, glucosides, acetylglucosides and malonylglucosides as major compounds was identified and quantified from 14 selected soybean seeds. Among them, genistein 7-O-(2"-O-apiosyl)glucoside and genistein 7-O-(6"-O-apiosyl)glucoside(ambocin) were identified tentatively as novel compounds in soybean seeds. Besides, among malonylglucosides, glycitein 4'-O-(6"-O-malonyl)glucoside was estimated for the first time. Total isoflavone contents were distributed from 240.21 to 445.21(mg/100 g, dry matter) and 7-O-6"-O-malonylglucosides were composed of 77.8% on total isoflavone as well as genistein derivatives were confirmed as major class. It was considered importantly that the development of isoflavone-rich varieties was necessary to strengthen their effects such as anti-inflammation, anti-cancer and menopause mitigation. The qualitative and quantitative data presented precisely in this study could be help to select and breed isoflavone-rich varieties. Furthermore, their basic isoflavone profile is expected to be applied to estimate the change of isoflavone conjugates on bioavailability after soy food supplements.

Speed-dependent Emission Characteristics of the Hazardous Air Pollutants from Diesel Medium-duty Trucks according to Emission Standards (배출허용기준 강화에 따른 차속별 경유 중형트럭의 유해대기오염물질 배출특성)

  • Hong, Heekyoung;Jung, Sungwoon;Son, Jihwan;Moon, Taeyoung;Lee, Sangeun;Moon, Sunhee;Yoon, Hyunjin;Kim, Jeongsoo;Kim, Jounghwa
    • Journal of ILASS-Korea
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    • v.20 no.2
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    • pp.121-129
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    • 2015
  • This study was designed to investigate the emission characteristics of unregulated pollutants (Aldehyde, VOCs, PAHs) as well as regulated pollutants (CO, HC, NOx and PM) from diesel medium-duty trucks. The emission characteristics of unregulated and regulated pollutants were assessed based on regulation standards (EURO 4 and EURO 5) and intake weight (2.5 ton and 5 ton). The results show that unregulated and regulated pollutants remained almost unchanged at higher speeds but decreased at below 23.5 km/h. Reduction in unregulated and regulated pollutants was noticeable in vehicles of recent regulation standards and light intake weight. The analysis of aldehyde using UPLC showed that formaldehyde and acetaldehyde of aldehyde were most dominant. The GC/MS analysis showed that benzene, toluene, ethylbenzene and xylene of VOCs was over 80% followed by toluene, xylene, ethylbenzene and benzene. In addition, the analysis of PAHs using GC/TOF-MS indicated that bi- and tricyclic aromatic ring of aromatic compounds was 73% and 53% at 2.5 ton and 5 ton vehicles, respectively. The results of this study will be contributed to establish HAPs inventory.

Analysis of antibiotic residues in milk from healthy dairy cows treated with bovine mastitis ointment using ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry

  • Park, Eun-Kee;Ryu, Yong-Jae;Cha, Chun-Nam;Yoo, Chang-Yeul;Kim, Suk;Lee, Hu-Jang
    • Korean Journal of Veterinary Research
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    • v.56 no.4
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    • pp.233-239
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    • 2016
  • This study was conducted to analyze penicillin G (PEG), streptomycin (STR) and neomycin (NEO) residues in milk of healthy lactating cows. Milk samples were collected from all four quarters of 12 dairy cows 2−7 days after intramammary infusions of an ointment containing PEG, STR and NEO once (n = 4; group I) or twice (n = 4, group II) daily. Ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry was used to determine the antibiotic residues in the samples. The correlation coefficient ($r^2$) of the calibration curves for all antibiotics was > 0.999 and the limits of detection and quantification were $0.002-0.005{\mu}g/mL$ and $0.007-0.02{\mu}g/mL$, respectively. Recovery rates were ranged from 75.5 to 92.3%. In group I, PEG, STR and NEO residues were detected in milk at 2, 3 and 2 days post-treatment, respectively, which were below the maximum residue limit (MRL). In group II, PEG, STR and NEO residues were detected in milk at 2, 3 and 3 days post-treatment, respectively, which were bellow the MRL. These results suggest that a 3-day for milk withdrawal period after the ointment treatment might be sufficient for reduction of the antibiotic residues below the MRL.

Remarkable impact of steam temperature on ginsenosides transformation from fresh ginseng to red ginseng

  • Xu, Xin-Fang;Gao, Yan;Xu, Shu-Ya;Liu, Huan;Xue, Xue;Zhang, Ying;Zhang, Hui;Liu, Meng-Nan;Xiong, Hui;Lin, Rui-Chao;Li, Xiang-Ri
    • Journal of Ginseng Research
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    • v.42 no.3
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    • pp.277-287
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    • 2018
  • Background: Temperature is an essential condition in red ginseng processing. The pharmacological activities of red ginseng under different steam temperatures are significantly different. Methods: In this study, an ultrahigh-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry was developed to distinguish the red ginseng products that were steamed at high and low temperatures. Multivariate statistical analyses such as principal component analysis and supervised orthogonal partial least squared discrimination analysis were used to determine the influential components of the different samples. Results: The results showed that different steamed red ginseng samples can be identified, and the characteristic components were 20-gluco-ginsenoside Rf, ginsenoside Re, ginsenoside Rg1, and malonyl-ginsenoside Rb1 in red ginseng steamed at low temperature. Meanwhile, the characteristic components in red ginseng steamed at high temperature were 20R-ginsenoside Rs3 and ginsenoside Rs4. Polar ginsenosides were abundant in red ginseng steamed at low temperature, whereas higher levels of less polar ginsenosides were detected in red ginseng steamed at high temperature. Conclusion: This study makes the first time that differences between red ginseng steamed under different temperatures and their ginsenosides transformation have been observed systematically at the chemistry level. The results suggested that the identified chemical markers can be used to illustrate the transformation of ginsenosides in red ginseng processing.

Botrytis cinerea hypovirulent strain △BcSpd1 induced Panax ginseng defense

  • Shuhan Zhang;Junyou Han;Ning Liu;Jingyuan Sun;Huchen Chen;Jinglin Xia;Huiyan Ju;Shouan Liu
    • Journal of Ginseng Research
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    • v.47 no.6
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    • pp.773-783
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    • 2023
  • Background: Gray mold, caused by Botrytis cinerea, is one of the major fungal diseases in agriculture. Biological methods are preferred over chemical fungicides to control gray mold since they are less toxic to the environment and could induce the resistance to pathogens in plants. In this work, we try to understand if ginseng defense to B. cinerea could be induced by fungal hypovirulent strain △BcSpd1. BcSpd1 encodes Zn(II)2Cys6 transcription factor which regulates fungal pathogenicity and we recently reported △BcSpd1 mutants reduced fungal virulence. Methods: We performed transcriptomic analysis of the host to investigate the induced defense response of ginseng treated by B. cinerea △BcSpd1. The metabolites in ginseng flavonoids pathway were determined by UPLC-ESI-MS/MS and the antifungal activates were then performed. Results: We found that △BcSpd1 enhanced the ginseng defense response when applied to healthy ginseng leaves and further changed the metabolism of flavonoids. Compared with untreated plants, the application of △BcSpd1 on ginseng leaves significantly increased the accumulation of p-coumaric acid and myricetin, which could inhibit the fungal growth. Conclusion: B. cinerea △BcSpd1 could effectively induce the medicinal plant defense and is referred to as the biological control agent in ginseng disease management.