• Title/Summary/Keyword: ESI MS

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Chemical Constituents from Aegle marmelos Fruits

  • Kim, Hye Jin;Seo, Young Ju;Htwe, Khin Myo;Yoon, Kee Dong
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.240-244
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    • 2021
  • Aegle marmelos (Rutaceae) is a deciduous shrub or tree and typically known as bael throughout Southeast Asia and has been used as a medicinal plant and a food ingredient. In this study eight compounds were determined to be O-(3,3-dimethylallyl) halfordinol (1), (R)-aegeline (2), (R)-marmeline (3), imperatorin (4), xanthotoxol (5), valencic acid (6), vanillic acid (7) and rutin (8). The chemical structures of the isolates were elucidated through spectroscopic evidence including 1D, 2D NMR, ESI-Q-TOF-MS and optical rotation.

Meliasendanins E-J, Nor-neolignan Constituents from Melia toosendan and their Anti-inflammatory Activity

  • Jin Woo Lee
    • Natural Product Sciences
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    • v.29 no.1
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    • pp.17-23
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    • 2023
  • A phytochemical investigation of the fruits extract of Melia toosendan afforded the isolation of two new nor-neolignans, meliasendanins E (1) and F (2), as well as twelve known compounds (3 - 14) using various separation technique such as Diaion HP20, silica, RP-18 gel column chromatography and semi-preparative HPLC. Their chemical structures were elucidated by extensive NMR spectroscopic data including 2D-NMR, and HR-ESI-MS as well as ECD data. Among the twelve known compounds, the absolute structures of 3 - 6 were determined first, and given the trivial names as meliasendanins G-J (3 - 6). Based on the evaluation of anti-inflammatory activity, compounds 7 - 8 exhibited inhibitory effects on LPS-induced nitric oxide production in RAW 264.7 macrophages with IC50 values of 34.6 and 39.5 µM, respectively.

Accurate determination of chloramphenicol in meat by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS) (동위원소희석 액체크로마토그래피-질량분석법을 이용한 육류 중 클로람페니콜의 정밀한 정량 분석에 관한 연구)

  • Song, Hye-Min;Kim, Byung-Joo;Jeong, Hyuk;Ahn, Seong-Hee
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.524-530
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    • 2010
  • Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

Purification and Structural Analysis of Surfactin Produced by Endophytic Bacillus subtilis EBS05 and its Antagonistic Activity Against Rhizoctonia cerealis

  • Wen, Cai-Yi;Yin, Zhi-Gang;Wang, Kai-Xuan;Chen, Jian-Guang;Shen, Shun-Shan
    • The Plant Pathology Journal
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    • v.27 no.4
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    • pp.342-348
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    • 2011
  • Bacillus subtilis EBS05, an endophytic bacteria strain isolated from a medicinal plant Cinnamomum camphor, can produce antagonistic compounds that effectively inhibit plant pathogenic fungi. The greenhouse experiments showed that wheat sharp eyespot disease (WSED) was reduced by 91.2%, 88.2% and 43.0% after the treatment with fermentation broth, bacteria-free filter and a fungicide fludioxonil, respectively. The culture broth of strain EBS05 can more effectively control WSED than can fludioxonil. The fermentation broth and bacteria-free filter ability to suppress WSED was not significantly different, suggesting that an active secreted substance played a major role in controlling WSED. Separation and purification of the active compounds was carried out by serial processes, including hydrochloric acid (pH 2.0) treatment, methanol extraction and Sephadex LH-20 column chromatography, silica gel column chromatography and reverse-phase high-pressure liquid chromatography (HPLC), respectively. The purified compounds, one of active peaks in the HPLC spectrum, were obtained from the collection. Analysis of the chemical structures by time-of-flight mass spectrometry (TOF-MS) and electrospray ionization mass spectrometry/mass spectrometry (ESI-MS/MS) showed that the active substances produced by the endophytic bacteria EBS05 are mixture of the ${\beta}$-hydroxy-C12~C15-$Leu^7$ surfactin A isomers with 1035.65 Da, 1021.64 Da, 1007.63 Da and 993.65 Da molecular weights, respectively.

Effects of Qi Gong Exercise on the Immune Response, Pulse Wave Parameter and Heart Rate Variability(HRV) for Post Mastectomy Women (기공(氣功) 운동이 유방암 절제술 여성의 면역, 맥상파 및 심박변이에 미치는 영향)

  • Kim, Yi Soon;Lee, Jeong Won;Kim, Yun Hee;Oh, Mi Jung;Kim, Gyeong Cheol
    • The Journal of the Society of Korean Medicine Diagnostics
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    • v.19 no.2
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    • pp.75-90
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    • 2015
  • Objectives The purposes of this study was to develope a Qi gong exercise that suits characteristics of post mastectomy women, and to evaluate the effect of Qi gong exercise on immune response, blood circulation index, pulse wave parameter and heart rate variability. Methods This study was applied to total 35 post mastectomy women, including 17 for experiment group and 18 for control group. The Qi gong exercise was composed of total 24 times of 90 minutes per each time, twice a week, and 12 weeks and it was conducted by the oriental medicine professor who was an expert of Qi gong exercise. Results 1. Two group comparison revealed that the experimental group had significantly improved immune response(p<.021), HR(beats/min)(p<.001), ESV(ml/beat)(p=.038), ESI($ml/beat/m^2$)(p=.040), ECO (L/min)(p=.019), ECI($L/min/m^2$)(p=.023), ECRI($dyne^*sec/cm$)(p=.015), Left Kwan($div^3$)(p=.021), Right Kwan($div^3$)(p=.038), Mean HRV(cycle/min)(p<.001), SDNN(ms)(p=.043), RMSSD(ms)(p=.040), and TP(log $ms^2$)(p=.039). 2. Two group comparison revealed that the experimental group had significantly decreased ECR ($dyne^*sec^*cm^{-5}$) (p=.034), Left RAI(p=.044), Right RAI(p=.042), and pNN50(%)(p=.038). Conclusions These results from Qi gong exercise program can be used as basic data for development of health promotion program for Post Mastectomy Women.

Study on Chemical Components of the Aerial Parts and the Roots of Buckwheat

  • Ham, Young-Min;Hyun, Ho-Bong;Yoon, Seon-A;Yoon, Weon-Jong;Yang, Woo-Sam;Oh, Dae-Ju
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2018.04a
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    • pp.61-61
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    • 2018
  • Buckwheat is a important vegetable in asia for long time. Recently, Buckwheat has attracted attention to its potential for health benefit and especially as a gluten-free food. Conventional buckwheat studies have focused on seeds and sprouts, but we studied the components of the aerial parts and roots of buckwheat after harvesting. Therefore, we hope that this research will be a basic study to expand the application range of buckwheat plants which are discarded after harvesting. The ethanol extracts of aerial part and roots of buckwheat (Daegwan, Yangjul) were analysed using high performance liquid chromatography (HPLC). Rutin was detected as the major compound in Daegwan, Yangjul aerial part and Daegwan root extracts, except yangjul root extract. So we analysed Yangjul root extract using liquid chromatography-mass spectrometry (LC-MS) and then obtained the informations about the components in Yangjul root extract. Yangjul root extract was analysed by $LC-MS^n$ in negative ESI mode within the range m/z 150-2000 amu. Totally, four components was found in the Yangjul root extract and obtained the fragments ion patterns of ones. Further study, we have to confirm the structure of components in Yangjul root extract and try to more biological activity test the components for development as useful food or cosmetic ingredients.

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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.

Identification of Glutathione Conjugates of 2, 3-Dibromopropene in Male ICR Mice

  • Lee Sang Kyu;Baik Seo Yeon;Jeon Tae Won;Jun In Hye;Kim Ghee Hwan;Jin Chun Hua;Lee Dong Ju;Kim Jun Kyou;Yum Young Na;Jeong Tae Cheon
    • Archives of Pharmacal Research
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    • v.29 no.2
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    • pp.172-177
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    • 2006
  • Hepatotoxic potential of 2, 3-dibromopropene (2, 3-DBPE) and its conjugation with glutathione (GSH) were investigated in male ICR mice. Treatment of mice with 20, 50, and 100 mg/kg of 2, 3-DBPE for 24 h caused elevation of serum alanine aminotransferase and aspartate aminotransferase activities. The hepatic content of GSH was not changed by 2, 3-DBPE. Meanwhile, the GSH content was slightly reduced when mice were treated with 2, 3-DBPE for 6 h and significantly increased 12 h after the treatment. Subsequently, a possible formation of GSH conjugate of 2, 3-DBPE was investigated in vivo. After the animals were treated orally with 20, 50, and 100 mg/kg of 2, 3-DBPE, the animals were subjected to necropsy 6, 12, and 24 h later. A conjugate of S-2-bromopropenyl GSH was identified in liver and serum treated with 100 mg/kg of 2, 3-DBPE by using liquid chromatography-electrospray ionization tandem mass spectrometry. The protonated molecular ions $[M+H]^+$ of S-2-bromopropenyl GSH were observed at m/z 425.9 and 428.1 in the positive ESI spectrum with a retention time of 6.35 and 6.39 min, respectively. In a time-course study in livers following an oral treatment of mice with 100 mg/kg of 2, 3-DBPE for 6, 12, and 24 h, the 2, 3-DBPE GSH conjugate was detected maximally 6 h after the treatment. The present results suggested that 2, 3-DBPE-induced hepatotoxicity might be related with the production of its GSH conjugate.

Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
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    • v.53 no.1
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    • pp.25-30
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    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

Optimization of solid-phase extraction for the liquid chromatography-tandem mass spectrometry analysis of basic drugs in equine urine (액체크로마토그래피-텐덤질량분석법을 위한 경주마 소변 중 염기성 약물의 고체상 추출법 최적화)

  • Shin, Hyun Du;Yang, Ji Suk;Jung, Mihye;Kim, Hyung-Seung;Youm, Jeong-Rok;Hu, Man Bae;Kim, Sung Jean;Han, Sang Beom
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.412-423
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    • 2008
  • A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.