• Title/Summary/Keyword: Ionization rate

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Determination of Residual Erythromycin Antibiotic in Fishery Products by Liquid Chromatography-electrospray Ionization Mass Spectrometry (LC-MS/MS를 이용한 어류 및 갑각류의 잔류 Erythromycin 항생제 분석)

  • Jo, Mi-Ra;Mok, Jong-Soo;Lee, Doo-Seog;Kim, Min-Jung;Kim, Poong-Ho
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.42 no.1
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    • pp.15-19
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    • 2009
  • A simple and sensitive method for erythromycin quantification by liquid chromatography electrospray mass spectrometry (LC-MS/MS) in fishery products was developed. Samples were extracted by liquid-liquid extraction using 70% acetonitrile. Lipids were removed by acetonitrile saturated hexane. LC separation was performed on a Shiseido UG C-18 column ($150\;mm{\times}2.0\;mm$ internal diameter.) with a gradient system of 0.2% acetic acid-acetonitrile containing 0.2% acetic acid as a mobile phase at flow rate of 0.2 mL/min. The mass spectrometer was operated in selected reaction monitoring with positive electro-spray interface. Transitions were monitored a m/z $734{\to}577$ and $734{\to}158$, with m/z $734{\to}577$ chosen for quantification. Recovery of erythromycin from fish and shrimp fortified at the 10 ng/mL, 50 ng/mL and 100 ng/mL were 91.6-109.4%, 84.4-111.2% and 98.8-109.6% with high precision, respectively. Limits of quantification and limits of detection of erythromycin in both fish and shrimp were 10.0 ng/mL and 1.0 ng/mL, respectively. This analysis method for erythromycin has been proposed for registration in the Korean Official Methods of Food Analysis and has been utilized for fishery products analysis by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.

Dosimetric Characteristic of Digital CCD Video Camera for Radiation Therapy

  • Young Woo. Vahc;Kim, Tae Hong.;Won Kyun. Chung;Ohyun Kwon;Park, Kyung Ran.;Lee, Yong Ha.
    • Progress in Medical Physics
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    • v.11 no.2
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    • pp.147-155
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    • 2000
  • Patient dose verification is one of the most important parts in quality assurance of the treatment delivery for radiation therapy. The dose distributions may be meaningfully improved by modulating two dimensional intensity profile of the individual high energy radiation beams In this study, a new method is presented for the pre-treatment dosimetric verification of these two dimensional distributions of beam intensity by means of a charge coupled device video camera-based fluoroscopic device (henceforth called as CCD-VCFD) as a radiation detecter with a custom-made software for dose calculation from fluorescence signals. This system of dosimeter (CCD-VCFD) could reproduce three dimensional (3D) relative dose distribution from the digitized fluoroscopic signals for small (1.0$\times$1.0 cm$^2$ square, ø 1.0 cm circular ) and large (30$\times$30cm$^2$) field sizes used in intensity modulated radiation therapy (IMRT). For the small beam sizes of photon and electron, the calculations are performed In absolute beam fluence profiles which are usually used for calculation of the patient dose distribution. The good linearity with respect to the absorbed dose, independence of dose rate, and three dimensional profiles of small beams using the CCD-VCFD were demonstrated by relative measurements in high energy Photon (15 MV) and electron (9 MeV) beams. These measurements of beam profiles with CCD-VCFD show good agreement with those with other dosimeters such as utramicro-cylindrical (UC) ionization chamber and radiographic film. The study of the radiation dosimetric technique using CCD-VCFD may provide a fast and accurate pre-treatment verification tool for the small beam used in stereotactic radiosurgery (SRS) and can be used for verification of dose distribution from dynamic multi-leaf collimation system (DMLC).

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Electrospray-Mass Spectrometric Analysis of Plasma Pyrophosphates Separated on a Multi-Modal Liquid Chromatographic Column

  • Lee, Su-Hyeon;Lee, Jeong-Ae;Lee, Won-Yong;Chung, Bong-Chul;Choi, Man-Ho
    • Mass Spectrometry Letters
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    • v.2 no.4
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    • pp.92-95
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    • 2011
  • Pyrophosphates are the key intermediates in the biosynthesis of isoprenoids, and their concentrations could reveal the benefits of statins in cardiovascular diseases. Quantitative analysis of five pyrophosphates, including isopentenyl pyrophosphate (IPP), dimethylallyl pyrophosphate (DMAPP), geranyl pyrophosphate (GPP), farnesyl pyrophosphate (FPP), and geranylgeranyl pyrophosphate (GGPP), was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative ionization mode. After dilution with methanol, samples were separated on a 3 ${\mu}m$ particle multi-modal $C_{18}$ column ($50{\times}2$ mm) and quantified within 10 min. The gradient elution consists of 10 mM ammonium bicarbonate and 0.5% triethylamine (TEA) in water and 0.1% TEA in 80% acetonitrile was used at the flow rate of 0.4 mL/min. Overall recoveries were 51.4-106.6%, while the limit of quantification was 0.05 ${\mu}g$/mL for GPP and FPP and 0.1 ${\mu}g$/mL for IPP, DMAPP, and GGPP. The precision (% CV) and accuracy (% bias) of the assay were 1.9-12.3% and 89.6-111.8%, respectively, in 0.05-10 ${\mu}g$/mL calibration ranges ($R^2$ > 0.993). The devised LC-MS/MS technique with the multi-modal $C_{18}$ column can be used to estimate the biological activity of pyrophosphates in plasma and may be applicable to cardiovascular events with cholesterol metabolism as well as the drug efficacy of statins.

Quantitative Determination and Antioxidant Effects of Cheonwangbosimdan (LC-MS/MS를 이용한 천왕보심단(天王補心丹)의 함량분석 및 항산화 효능 연구)

  • Seo, Chang-Seob;Kim, Ohn Soon;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.45 no.4
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    • pp.300-314
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    • 2014
  • An ultra-performance liquid chromatography-electrospray ionization-mass spectrometer (UPLC-ESI-MS) method was established for the simultaneous quantification of eighteen marker compounds in traditional Korean formula, Cheonwangbosimdan (CWBSD). In addition, we evaluated the antioxidant effects of CWBSD. Eighteen marker components were separated on a UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and kept at $45^{\circ}C$ by gradient elution with 0.1% (v/v) formic acid in water and acetonitrile as mobile phase. The flow rate was 0.3 mL/min and the injection volume was $2.0{\mu}L$. The antioxidant activities of CWBSD were assessed by measuring free radical scavenging activities on 2,2'-azinobis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The calibration curves of all analytes showed good linearity (correlation coefficient ${\geq}0.9937$) within the test ranges. The limits of detection and quantification for the 18 marker compounds were 0.01-4.71 ng/mL and 0.03-14.13 ng/mL, respectively. The contents of the 18 compounds in CWBSD extract ranged from none to $1701.00{\mu}g/g$. The CWBSD showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction ($RC_{50}$) against ABTS and DPPH radicals were $149.42{\mu}g/mL$ and $339.24{\mu}g/mL$.

Quantitative Analysis of the Fifteen Constituents in Hyangso-San by LC-MS/MS (LC-MS/MS를 이용한 향소산 중 15종 성분의 정량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.47 no.4
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    • pp.381-388
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    • 2016
  • Hyangso-san is a traditional herbal medicine that consists of the seven herbal medicines, Cyperi Rhizoma, Perillae Folium, Atractylodis Rhizoma, Citri Unshius Pericarpium, Glycyrrhizae Radix et Rhizoma, Zingiberis Rhizoma Crudus, and Allii Fistulosi Bulbus. Hyangso-san has long been clinically used to treat the influenza, including headache, ferver, chills, and pantalgia. In this study, we were performed the simultaneous analysis of the 15 marker compounds (liquiritin apioside, liquiritin, ferulic acid, naringin, hesperidin, rosmarinic acid, liquiritigenin, kaempferol, glycyrrhizin, nobiletin, 6-gingerol, elemicin, atractylenolide III, nootkatone, and atractylenolide I) in Hyangso-san using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS). Column for the separation of the 15 ingredients was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ by using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient condition. Identifications of all analytes were performed using a Waters ACQUITY TQD LC-MS/MS system. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. Correlation coefficient of the calibration curve was ${\geq}0.9958$. The values of limits of detection and quantification of the 15 components were 0.002-4.29 and 0.01-12.88 ng/mL, respectively. The result of an analysis using the established LC-MS/MS method, kaempferol and atractylenolide I were not detected, while other 13 compounds were 0.08-56.87 mg/g in lyophilized Hyangso-san sample.

Optical and Electrical Properties of Fluorine-Doped Tin Oxide Prepared by Chemical Vapor Deposition at Low Temperature (저온 증착된 불소도핑 주석 산화 박막의 광학적·전기적 특성)

  • Park, Ji Hun;Jeon, Bup Ju
    • Korean Journal of Materials Research
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    • v.23 no.9
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    • pp.517-524
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    • 2013
  • The electrical and optical properties of fluorine-doped tin oxide films grown on polyethylene terephthalate film with a hardness of 3 using electron cyclotron resonance plasma with linear microwave of 2.45 GHz of high ionization energy were investigated. Fluorine-doped tin oxide films with a magnetic field of 875 Gauss and the highest resistance uniformity were obtained. In particular, the magnetic field could be controlled by varying the distribution in electron cyclotron deposition positions. The films were deposited at various gas flow rates of hydrogen and carrier gas of an organometallic source. The surface morphology, electrical resistivity, transmittance, and color in the visible range of the deposited film were examined using SEM, a four-point probe instrument, and a spectrophotometer. The electromagnetic field for electron cyclotron resonance condition was uniformly formed in at a position 16 cm from the center along the Z-axis. The plasma spatial distribution of magnetic current on the roll substrate surface in the film was considerably affected by the electron cyclotron systems. The relative resistance uniformity of electrical properties was obtained in film prepared with a magnetic field in the current range of 180~200A. SEM images showing the surface morphologies of a film deposited on PET with a width of 50 cm revealed that the grains were uniformly distributed with sizes in the range of 2~7 nm. In our experimental range, the electrical resistivity of film was able to observe from $1.0{\times}10^{-2}$ to $1.0{\times}10^{-1}{\Omega}cm$ where optical transmittance at 550 nm was 87~89 %. These properties were depended on the flow rate of the gas, hydrogen and carrier gas of the organometallic source, respectively.

Effectiveness of Bioremediation on Oil-Contaminated Sand in Intertidal Zone

  • Oh, Young-Sook;Sim, Doo-Suep;Kim, Sang-Jin
    • Journal of Microbiology and Biotechnology
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    • v.13 no.3
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    • pp.437-443
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    • 2003
  • Bioremediation technologies were applied to experimental microcosms, simulating an oil spill in a lower intertidal area. Three treatments (oil only, oil plus nutrients, and oil plus nutrients and microbial inocula) were applied, and each microcosm was repeatedly filled and eluted with seawater every 12 h to simulate tidal cycles. To minimize washing-out of the inoculum by the tidal cycles, microbial cells were primarily immobilized on diatomaceous earth before they were applied to the oiled sand. Oil degradation was monitored by gravimetric measurements, thin layer chromatography/flame ionization detector (TLC/FID) analysis, and gas chromatography (GC) analysis, and the loss of oil content was normalized to sand mass or nor-hopane. When the data were normalized to sand mass, no consistent differences were detected between nutrient-amended and nutrient/inoculum-amended microcosms, although both differed from the oil-only microcosm in respect of oil removal rate by a factor of 4 to 14. However, the data relative to nor-hopane showed a significant treatment difference between the nutrient-amended and nutrient/inoculum-treated microcosms, especially in the early phase of the treatment. The accelerating effect of inoculum treatment has hardly been reported in studies of oil bioremediation in the Tower intertidal area. The inoculum immobilized on diatomaceous earth seemed to be a very effective formulation for retaining microbial cells in association with the sand. Results of this study also suggest that interpretation of the effectiveness of bioremediation could be dependent on the selection of monitoring methods, and consequently the application of various analytical methods in combination could be a solution to overcome the limitations of oil bioremediation monitoring.

Antifungal Effect of Triglycerol Monolaurate Synthesized by Lipozyme 435-Mediated Esterification

  • Zhang, Song;Xiong, Jian;Lou, Wenyong;Ning, Zhengxiang;Zhang, Denghui;Yang, Jiguo
    • Journal of Microbiology and Biotechnology
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    • v.30 no.4
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    • pp.561-570
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    • 2020
  • This study was designed to synthesize triglycerol monolaurate (TGML) with Lipozyme 435 as the catalyst, and explore its effects on the growth of Aspergillus parasiticus (A. parasiticus) and Aspergillus flavus (A. flavus) and the secretion of aflatoxin b1. The highest content of TGML (49.76%) was obtained at a molar ratio of triglycerol to lauric acid of 1.08, a reaction temperature of 84.93℃, a reaction time of 6 h and an enzyme dosage of 1.32%. After purification by molecular distillation combined with the washes with ethyl acetate and water, the purity of TGML reached 98.3%. Through characterization by electrospray-ionization mass spectrometry, infrared spectrum and nuclear magnetic resonance, the structure of TGML was identified as a linear triglycerol combined with lauroyl at the end. Finally, the inhibitory effects of TGML on the growths of A. parasiticus and A. flavus and the secretion of aflatoxin b1 were evaluated by measuring the colony diameter, the inhibition rate of mycelial growth and the content of mycotoxin in the media. The results indicated that TGML had a stronger inhibitory effects on colony growth and mycelial development of both toxic molds compared to sodium benzoate and potassium sorbate, and the secretions of toxins from A. parasiticus and A. flavus were completely suppressed when adding TGML at 10 and 5 mM, respectively. Based on the above results, TGML may be used as a substitute for traditional antifungal agents in the food industry.

Quantitative Evaluation of Radix Astragali through the Simultaneous Determination of Bioactive Isoflavonoids and Saponins by HPLC/UV and LC-ESI-MS/MS

  • Kim, Jin-Hee;Park, So-Young;Lim, Hyun-Kyun;Park, Ah-Yeon;Kim, Ju-Sun;Kang, Sam-Sik;Youm, Jeong-Rok;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.28 no.7
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    • pp.1187-1194
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    • 2007
  • The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. These methods were fully validated with respect to the linearity, accuracy, precision, recovery and robustness. The HPLC/UV method was applied successfully to the quantification of three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

Deposition Characteristic of InNx Films by Reactive DC Magnetron Sputtering (반응성 직류 스퍼터법에 의한 질화 인듐 박막의 제막 특성)

  • 송풍근;류봉기;김광호
    • Journal of the Korean Ceramic Society
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    • v.40 no.8
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    • pp.739-745
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    • 2003
  • In $N_{x}$ films were deposited on soda-lime glass without substrate heating by reactive dc magnetron sputtering using indium (In) metal target. Depositions were carried out under various total gas pressures ( $P_{tot}$) of mixture gases (Ar+$N_2$ or He+$N_2$). He gas was introduced to $N_2$ gas in order to enhance the reactivity of nitrogen on film surface by the "penning ionization". Plasma impedance decreased greatly when 20% or more introduced the $N_2$ gas. This is due to the In $N_{x}$ layers formed on target surface because a secondary electron emission rate of InN is small compared with In metal. XRD patterns of the films revealed that <001> preferred oriented polycrystalline In $N_{x}$ films, where the crystallinity of the films was improved with decrease of $P_{tot}$ and with increase of $N_2$ flow ratio. The improvement of the crystallinity and stoichimetry of the In $N_{x}$ films were considered to be caused by an increase in the activated nitrogen radicals and also by an increase in the kinetic energy of sputtered In atoms arriving at growing film surface, which should enhance the chemical reaction and surface migration on the growing film surface, respectively. Furthermore, the films deposited using mixture gases of He+$N_2$ showed higher crystallinity compared with the film deposited by the mixture gases of Ar+$N_2$.$.EX>.