• Title/Summary/Keyword: LC-QTOF-MS

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Bioassay-coupled LC-QTOF MS/MS to Characterize Constituents Inhibiting Nitric Oxide Production of Thuja orientalis

  • Park, Dawon;Shin, Hyeji;Byun, Youngjoo;Lee, Ki Yong
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.293-299
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    • 2021
  • The ethyl acetate fractions prepared from the leaves of Thuja orientalis significantly inhibited nitric oxide (NO) production in lipopolysaccharide-stimulated BV2 microglial cells. According to bioassay-coupled LC-QTOF MS/MS, the components near 22 and 25 mins in the mass chromatogram highly inhibited NO production and were expected to be labdane diterpenes, and the active components were characterized via further isolation. The results of the NO production inhibitory assay of the isolated compounds correlated well with the results of bioassay-coupled LC-QTOF MS/MS. Among the identified constituents, NO production inhibitory activities of 16-hydroxy-labda-8(17),13-diene-15,19-dioic acid butenolide (2) and 15-hydroxypinusolidic acid (3) were newly reported. Taken together, these results demonstrated that LC-QTOF MS/MS coupled with NO production inhibition assay was a powerful tool for accurately predicting new anti-inflammatory constituents in the extracts from natural products. Moreover, it provided a potential basis for broadening the application of bioassay-coupled LC-QTOF MS/MS in natural product research.

Identification and evaluation of fragmentation pathways of PDE-5 inhibitor analogues using LC-QTOF-MS (LC-QTOF-MS를 이용한 발기부전치료제 유사물질의 fragmentation pathway 분석)

  • Do, Jung-Ah;Noh, Eunyoung;Yoon, Soon-Byung;Park, Hyoung-Joon;Cho, Sooyeul;Park, Sung-Kwan;Yoon, Chang-Yong
    • Analytical Science and Technology
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    • v.28 no.4
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    • pp.278-287
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    • 2015
  • Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction. In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatography-quadrupole-time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions. Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.

Metabolomics Investigation of Cutaneous T Cell Lymphoma Based on UHPLC-QTOF/MS

  • Zhou, Qing-Yuan;Wang, Yue-Lin;Li, Xia;Shen, Xiao-Yan;Li, Ke-Jia;Zheng, Jie;Yu, Yun-Qiu
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.13
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    • pp.5417-5421
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    • 2014
  • Objectives: The identification of cutaneous T cell lymphoma (CTCL) biomarkers may serve as a predictor of disease progression and treatment response. The aim of this study was to map potential biomarkers in CTCL plasma. Design and Methods: Plasma metabolic perturbations between CTCL cases and healthy individuals were investigated using metabolomics and ultrahigh performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF/MS). Results: Principal component analysis (PCA) of the spectra showed clear metabolic changes between the two groups. Thirty six potential biomarkers associated with CTCL were found. Conclusions: Based on PCA, several biomarkers were determined and further identified by LC/MS/MS analysis. All of these could be potential early markers of CTCL. In addition, we established that heparin as a nticoagulant has better pre-treatment results than EDTA with the UHPLC-QTOF/MS appraoch.

Ginsenosides analysis of New Zealand-grown forest Panax ginseng by LC-QTOF-MS/MS

  • Chen, Wei;Balan, Prabhu;Popovich, David G.
    • Journal of Ginseng Research
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    • v.44 no.4
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    • pp.552-562
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    • 2020
  • Background: Ginsenosides are the unique and bioactive components in ginseng. Ginsenosides are affected by the growing environment and conditions. In New Zealand (NZ), Panax ginseng Meyer (P. ginseng) is grown as a secondary crop under a pine tree canopy with an open-field forest environment. There is no thorough analysis reported about NZ-grown ginseng. Methods: Ginsenosides from NZ-grown P. ginseng in different parts (main root, fine root, rhizome, stem, and leaf) with different ages (6, 12, 13, and 14 years) were extracted by ultrasonic extraction and characterized by Liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. Twenty-one ginsenosides in these samples were accurately quantified and relatively quantified with 13 ginsenoside standards. Results: All compounds were separated in 40 min, and a total of 102 ginsenosides were identified by matching MS spectra data with 23 standard references or published known ginsenosides from P. ginseng. The quantitative results showed that the total content of ginsenosides in various parts of P. ginseng varied, which was not obviously dependent on age. In the underground parts, the 13-year-old ginseng root contained more abundant ginsenosides among tested ginseng samples, whereas in the aboveground parts, the greatest amount of ginsenosides was from the 14-year-old sample. In addition, the amount of ginsenosides is higher in the leaf and fine root and much lower in the stem than in the other parts of P. ginseng. Conclusion: This study provides the first-ever comprehensive report on NZ-grown wild simulated P. ginseng.

Quali-Quantitative Analysis of Flavonoids for Mulberry Leaf and Fruit of 'Suhyang'

  • Ju, Wan-Taek;Kwon, O-Chul;Lee, Min-Ki;Kim, Hyun-Bok;Sung, Gyoo-Byung;Kim, Yong-Soon
    • Korean Journal of Environmental Agriculture
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    • v.36 no.4
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    • pp.249-255
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    • 2017
  • BACKGROUND: Globally, mulberry (Morus sp.) is exploited for feeding leaf to silkworms in order to obtain silk fiber or for animal feedstock production. Also, mulberry fruit is known to a by-product that was produced from mulberry tree after harvesting leaves for silkworm rearing, as a yield and consumption of mulberry fruit was increased, it has been fixing to a newincome crop. Mulberry leaves and fruits are used for the health benefits of human beings. Mulberry contains various bioactive components, such as alkaloids and flavonoids. Mulberry flavonoids are an important part of the diet because of their effects on human nutrition. The flavonoids in mulberry leaf and fruit of 'Suhyang'(Morus alba L.) were determined. METHODS AND RESULTS: Flavonoids for mulberry leaf and fruit of 'Suhyang' were analysed using ultrahigh performance liquid chromatography coupled with diode array detection and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS)technique. An UPLC-DAD-QTOF/MS system was used, and identification of mulberry leaves constituents was carried out on the basis of the complementary information obtained from LC spectra, MS ions, and MS/MS fragments. The mulberry leaf (16 flavonoids) and fruit (9 flavonoids) were isolated and analyzed from Suhyang using UPLC-DAD-QTOF/MS chromatogram. To the best of our knowledge, Quercetin 3-O-(6"-O-malonyl) glucoside and quercetin 3-O-rutinoside (rutin) was detected on the highest content in leaf and fruit, respectively and further research will be devoted to evaluate their biological activity. CONCLUSION: Obtaining information about the concentration of functional materials in mulberry leaves could contribute to the development and promotion of processed, functional products and offer possible industrial use of 'Suhyang', holding promises to enhance the overall profitability of sericulture.

Purification and Identification of Cytotoxic Compounds from the Root of Rumex crispus L. (소리쟁이 뿌리로부터 세포독성물질 분리 및 정제)

  • Cho, Yong Beom;Kim, Jae Yeon;Kwon, Nam Woo;Hwang, Bang Yeon;Kim, Jun Gu;Woo, Sun Hee;Lee, Moon Soon
    • Korean Journal of Medicinal Crop Science
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    • v.27 no.3
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    • pp.208-217
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    • 2019
  • Background: In the present study, we identified two cytotoxic compounds from the root of Rumex crispus L. using a bioassay-based method. Methods and Results: Compared with the other fractions, the diethyl ether ($Et_2O$) fraction of R. crispus root extract exhibited the strongest of 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging effect [scavenging concentration 50% $(SC_{50})=63.8{\pm}1.47{\mu}g/m{\ell}$], nitric oxide (NO) production inhibitory effect on the mouse macrophage cell line RAW264.7 [inhibitory concentration 50% $(IC_{50})=60.9{\pm}7.52{\mu}g/m{\ell}$] and cytotoxicity effect on the human hepatoma cell line, HepG2 [lethal concentration 50% $(LC_{50})=115.4{\pm}1.86{\mu}g/m{\ell}$]. According to the bioassay-based method, two cytotoxic compounds were purified from the $Et_2O$ fraction by using column chromatography and preparative high performance liquid chromatography (prep-HPLC). These two compounds were identified as parietin and chrysophanol by using nuclear magnetic resonance (NMR) and liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS). In addition, both parietin and chrysophanol exhibited a cytotoxicity effect on HepG2 cells, their $LC_{50}$ values were $169.1{\pm}17.67{\mu}M$ and $111.5{\pm}6.62{\mu}M$, respectively. Conclusions: Parietin and chrysophanol isolated from the $Et_2O$ fraction of the R. crispus root extract showed cytotoxicity in HepG2 cell.

Analysis of antioxidant and anti-inflammatory effects of Mongolian wild lingonberry and blueberry, and identification of their bioactive compounds (몽골 야생 링곤베리와 블루베리의 항산화, 항염증 효과 및 생리활성 물질 분석 연구)

  • Lee, Hye Ju;Naranbulag, Batdorj;Jeong, Seung Jin;Seo, Chan;Lee, Sang-Gil
    • Korean Journal of Food Science and Technology
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    • v.54 no.2
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    • pp.147-154
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    • 2022
  • The Mongolian lingonberry and blueberry are two essential food sources found in Mongolia. This study investigated the antioxidant and anti-inflammatory effects of methanol extracts from Mongolian lingonberry (LBE) and blueberry (BBE). Compared to the LBE, the BBE showed higher total phenolic, flavonoid, and anthocyanin contents, as well as antioxidant capacities. The LBE and BBE inhibited the mRNA expression of pro-inflammatory genes, including tumor necrosis factor-α (TNF-α), interleukin-1β (IL-1β), and cyclooxygenase (COX-2) in lipopolysaccharide-stimulated RAW 264.7 macrophage cells. In addition, the LBE and BBE inhibited NADPH oxidase-2 (Nox2) mRNA expression, indicating that they have cellular antioxidant capacities. Anthocyanin derivatives of the LBE and BBE were analyzed using LC-QTOF/MS. Six anthocyanins were identified in the BBE, while one was detected in the LBE. Our findings demonstrate that the anthocyanin-rich LBE and BBE could be used as functional food sources in Mongolia.