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Isolation and Structural Identification of Antioxidant Substances from Ethyl Acetate Extract of Conyza canadensis (망초(Conyza canadensis) Ethyl Acetate 추출물의 항산화성 물질의 분리와 동정)

  • Hyun Sook Song
    • Journal of Naturopathy
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    • v.12 no.1
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    • pp.7-15
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    • 2023
  • Background: As a result of analyzing the components of wild Conyza canadensis, it contains physiologically active ingredients, so it is necessary to identify the compound. Purposes: It was to study the compound's molecular structure; a previous study showed that C. canadensis contains antioxidant substances. Methods: The ultrasonic pulverized lysate of C. canadensis stem and leaves was first extracted with 90% methanol and then five organic solvents. Next, the extracts was fractionated by HPLC, LC/MS chromatography, and NMR analyzers identified the molecular structure. Results: 100 g of dry C. canadensis was sonicated in 90% methanol and concentrated under reduced pressure to 11.96 g of a crude extract. Then, this crude was extracted with five types of solvents to obtain 123.8 mg of n-hexane, 448.2 mg of dichloromethane, 1047.7 mg of ethyl acetate (EA), 2563.8 mg of butanol, and 7.04 g of water. The EA extracts were fractionated by LC-MS and then re-fractionated to obtain F1 to F20. Next, the F15 was further fractionated to obtain nine fine fractions. Finally, the F17 fraction was re-fractionated to obtain ten fine fractions. As a result of LC-MS and NMR spectrometer analysis of the F15-7, the structure of this compound was confirmed as 3,5-dicaffeoylquinic acid. As a result of examining the structures of the F17-4 and F17-5 fractions, Quercetin-3-o-β-galactose was identified. In addition, the form of the F17-10 was confirmed to be 1,3,4-tri-caffeoylquinic acid. Conclusions: This study demonstrated that C. canadensis contained phenolic antioxidants, and its utilization may be expected.

Development of Reuse Process Through Recovery and Refinement of Precursor for LED (LED용 precursor 재이용을 위한 회수 및 정제 공정 개발)

  • Yang, Jae Yeol;O, Byung Sung;Yoon, Jae Sik
    • Resources Recycling
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    • v.23 no.1
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    • pp.25-32
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    • 2014
  • The purpose of this research is to develop a process and a system to collect, purify and reuse the residual quantity of trimethylgallium, used as a raw material, upon GaN epitaxial growth for LED from a metal organic chemical vapor deposition(MOCVD) equipment. This research reviews whether TMGa collected from the process can be used through a chemical and structural characteristics evaluation. As a result of analyzing the purity using ICP-MS and ICP-AES, 7N high purity (99.99999%) of TMGa was obtained. According to checking the structural change of TMGa through NMR analysis, TMGa having pure $(CH_3)_3Ga$ structure was obtained without structural change. For reliability review of the collected TMGa, u-GaN was deposited using the MOCVD process and an structural, optical and electrical characteristics evaluation was conducted. As a result, it was found out that the reuse was possible.

Isolation and Identification of Macamides from the Lipidic Extract of Maca [Lepidium meyenii] using Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 maca [Lepidium meyenii]의 지질 추출물로부터 macamides 분리 및 동정)

  • Lee, Seung-Ho;Kang, Jung-Il;Lee, Sang-Yun;Ha, Hyo-Cheol;Song, Young-Keun;Byun, Sang-Yo
    • KSBB Journal
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    • v.23 no.2
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    • pp.153-157
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    • 2008
  • Maca (Lepidium meyenii) has been used as a food and medicine in Peru for thousands of years. More recently a wide array of commercial maca products have gained popularity as dietary supplements with claims of anabolic and aphrodisiac effects. Even though the biologically active principles of maca are not fully known, the lipidic extract of maca tubers containing macamides showed promising physiological activities. In this study, the lipidic extract were collected from maca tubers by using supercritical carbon dioxide ($SCO_2$). Substance estimated as macamide in the extract was isolated and purified by preparative HPLC with recycling system. Two of the purified substance was identified as N-benzyl-5-oxo-6E,8E-octadecadienamide and N-benzylhexadecan amide by LC/MS, $^1H$-NMR and $^{13}C$-NMR analyses.

Development of Anther and Cell Culture Techniques for Enhancement of Rice Productivity (수도 생산성증대를 위한 화분세포 배양 및 융합기술 확립)

  • 허문회;채영암
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.29 no.3
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    • pp.232-241
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    • 1984
  • A series of experiments were carried out to know the effects of pollen stage, cold shock temperature and duration, and media for callus and green plant induction in rice anther culture. The results indicated that: (a) uninucleate stage of pollen was the most suitable stage for effective callus induction, (b) cold shock temperature of 8$^{\circ}C$ and 12$^{\circ}C$ was appeared to be proper temperature for callus induction, (c) callus induction rate was increased in the eight to 12 days long cold storage, (d) the medium N6 was better than that of N6D for callus induction, (e) green plant induction was better in both 4$^{\circ}C$ and 8$^{\circ}C$ than that of 12$^{\circ}C$ cold shock, (f) green plant frequency was higher in eight to 12 days long cold storage and (g) green plant frequency was doubled in the MS medium when compared with N6 medium.

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Electrosynthesis of n-PFOSF with Potential Operation (정전위법에 의한 n-PFOSF 합성)

  • Lee, Jongil;Tae, Beomseok
    • Applied Chemistry for Engineering
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    • v.7 no.3
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    • pp.473-480
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    • 1996
  • Synthesis of n-perfluorooctanesulfonyl fluoride(n-PFOSF), which is valuable precursor perfluoro-chemicals, was studied by electrochemical fluorination(ECF). Of prime concern was to investigate the cyclic voltamograms of Ni electrode in anhydrous hydrogen fluoride(AHF) with and without the reactants and to measure fluorine evolution potential. In a batch cell, chronoampherometric electrolysis and various chemical analysis such as GC, GC/MS and IR were used to understand the amphere change of electrode and the reaction paths. Fluorine equilibrium potential was found to be about 2.8V(vs. $Cu/CuF_2$) from the cyclic voltammograms and decay curves of anode potential in AHF. In batch processes, the ECF proceeded in two distinguished steps. The first step proceeded electrochemically and the second one chemically. Under 7V(vs. $Cu/CuF_2$), amount of crude products was proportional to the applied anode potential. Above 7V(vs. $Cu/CuF_2$), it had a hundred percentage with weight ratio of reactants and productivity of PFOSF was almost constant.

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Identification of N,N',N"-triacetylfusarinine C as a key metabolite for root rot disease virulence in American ginseng

  • Walsh, Jacob P.;DesRochers, Natasha;Renaud, Justin B.;Seifert, Keith A.;Yeung, Ken K.C.;Sumarah, Mark W.
    • Journal of Ginseng Research
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    • v.45 no.1
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    • pp.156-162
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    • 2021
  • Background: It is estimated that 20-30% of ginseng crops in Canada are lost to root rot each harvest. This disease is commonly caused by fungal infection with Ilyonectria, previously known as Cylindrocarpon. Previous reports have linked the virulence of fungal disease to the production of siderophores, a class of small-molecule iron chelators. However, these siderophores have not been identified in Ilyonectria. Methods: High-resolution LC-MS/MS was used to screen Ilyonectria and Cylindrocarpon strain extracts for secondary metabolite production. These strains were also tested for their ability to cause root rot in American ginseng and categorized as virulent or avirulent. The differences in detected metabolites between the virulent and avirulent strains were compared with a focus on siderophores. Results: For the first time, a siderophore N,N',N"-triacetylfusarinine C (TAFC) has been identified in Ilyonectria, and it appears to be linked to disease virulence. Siderophore production was suppressed as the concentration of iron increased, which is in agreement with previous reports. Conclusion: The identification of the siderophore produced by Ilyonectria gives us further insight into the root rot disease that heavily affects ginseng crop yields. This research identifies a molecular pathway previously unknown for ginseng root rot and could lead to new disease treatment options.

Characterization and screening of pyrrolizidine alkaloids by UPLC-MS/MS: Application to honey (UPLC-MS/MS를 이용한 벌꿀제품의 피롤리지딘 알칼로이드 잔류실태 및 분석법 선진화)

  • Ryu, Hoejin;Kim, Oukhee;Lee, Eunsoon;Kim, Misun;Kim, Jeong-gon;Yun, Eunsun;Kim, Hyunjeong;Kim, Musang
    • Analytical Science and Technology
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    • v.32 no.6
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    • pp.252-261
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    • 2019
  • Pyrrolizidine alkaloids (PAs) are a group of secondary metabolites that are produced by plants all over the world as a defense mechanism against herbivores. To date, over 660 PAs have been identified from more than 6,000 plant species that have been reported to be widely present in plants belonging to Asteraceae, Boraginaceae, and Fabaceae. This study describes an analytical method based on UPLC-MS/MS for the quantitation of 7 pyrrolizidine alkaloids (Lycopsamine, Echimidine, Retrorsine, Retrorsine N-oxide, Senecionine, Heliotrine, and Trichodesmine) in honey, and was applied to 84 honey samples for validation. Quantitation was performed based on a matrix-matched calibration to compensate for the matrix effect on the electrospray ionization. Good linear calibrations were obtained for all 7 PAs in the spiked honey samples (2.575-202.14 ㎍/kg; R2 ≥ 0.998). The extraction recoveries for most of the PAs in the honey samples were in the range of 81 %-108 %. The analysis showed that 6 of the 84 honey samples were contaminated by the PAs with the mean total sum of PAs being 47.19 ㎍/kg, and the concentrations of the PAs were observed to be in the range of 1.76-202.1 ㎍/kg. The retronecine type compounds (Echimidine, Lycopsamine) were the most frequently found PAs in honey. These data provide useful information for the assessment of human risk posed by the consumption of honey contaminated PAs.

A 12b 130MS/s 108mW $1.8mm^2$ 0.18um CMOS ADC for High-Quality Video Systems (고화질 영상 시스템 응용을 위한 12비트 130MS/s 108mW $1.8mm^2$ 0.18um CMOS A/D 변환기)

  • Han, Jae-Yeol;Kim, Young-Ju;Lee, Seung-Hoon
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.45 no.3
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    • pp.77-85
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    • 2008
  • This work proposes a 12b 130MS/s 108mW $1.8mm^2$ 0.18um CMOS ADC for high-quality video systems such as TFT-LCD displays and digital TVs requiring simultaneously high resolution, low power, and small size at high speed. The proposed ADC optimizes power consumption and chip area at the target resolution and sampling rate based on a three-step pipeline architecture. The input SHA with gate-bootstrapped sampling switches and a properly controlled trans-conductance ratio of two amplifier stages achieves a high gain and phase margin for 12b input accuracy at the Nyquist frequency. A signal-insensitive 3D-fully symmetric layout reduces a capacitor and device mismatch of two MDACs. The proposed supply- and temperature- insensitive current and voltage references are implemented on chip with a small number of transistors. The prototype ADC in a 0.18um 1P6M CMOS technology demonstrates a measured DNL and INL within 0.69LSB and 2.12LSB, respectively. The ADC shows a maximum SNDR of 53dB and 51dB and a maximum SFDR of 68dB and 66dB at 120MS/s and 130MS/s, respectively. The ADC with an active die area of $1.8mm^2$ consumes 108mW at 130MS/s and 1.8V.

Method Development for the Profiling Analysis of Urine Globotriaosylceramide (Gb3) for the Screening of Fabry Disease by Tandem Mass Spectrometry (ESI-MS/MS를 이용한 소변 중 Globotriaosylceramide(Gb3)의 정량 및 임상 응용; 패브리병(Fabry) 진단)

  • Yoon, Hye-Ran;Cho, Kyung-Hee;Kang, Seung-Woo;Kwon, Young-Joo;Jeong, Choon-Sik;Lee, Yong-Soo
    • YAKHAK HOEJI
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    • v.51 no.2
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    • pp.96-102
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    • 2007
  • Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in urine has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. A simple, rapid, and highly sensitive analytical method for Gb3 in urine was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Only simple 5-fold dilution of urine is necessary for the extraction and isolation of Gb3 in urine. Gb3 in diluted urine was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Eight isoforms of Gb3 were completely resolved from urine matrix. C24:0 Gb3 occupied 50% of total Gb3 as a major component in urine. Linear relationship for Gb3 isoforms was found in the range of 0.005${\sim}$5.0 ${\mu}$g/ml. The limit of detection (S/N=5) was 0.005 ${\mu}$g/ml and limit of quantification was 0.05 ${\mu}$g/ml for C24:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9598 to 0.9975. This method could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

Chromatographic Determination of the Absolute Configuration in Sanjoinine A That Increases Nitric Oxide Production

  • Soohyun Um;Hyeongju Jeong;Joon Soo An;Se Jin Jo;Young Ran Kim;Dong-Chan Oh;Kyuho Moon
    • Biomolecules & Therapeutics
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    • v.31 no.5
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    • pp.566-572
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    • 2023
  • A chiral derivatization strategy with phenylglycine methyl ester (PGME) was employed to develop a straightforward method to determine the absolute configurations of N,N-dimethyl amino acids. The PGME derivatives were analyzed using liquid chromatography-mass spectrometry to identify the absolute configurations of various N,N-dimethyl amino acids based on their elution time and order. The established method was applied to assign the absolute configuration of the N,N-dimethyl phenylalanine in sanjoinine A (4), a cyclopeptide alkaloid isolated from Zizyphi Spinosi Semen widely used as herbal medicine for insomnia. Sanjoinine A displayed production of nitric oxide (NO) in LPS-activated RAW 264.7 cells.