• Title/Summary/Keyword: MS solution

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Rapid separation and identification of 31 major saponins in Shizhu ginseng by ultra-high performance liquid chromatography-electron spray ionization-MS/MS

  • Sun, Ting-Ting;Liang, Xin-Lei;Zhu, He-Yun;Peng, Xu-Ling;Guo, Xing-Jie;Zhao, Long-Shan
    • Journal of Ginseng Research
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    • v.40 no.3
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    • pp.220-228
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    • 2016
  • Background: Among the various ginseng strains, Shizhu ginseng is endemic to China, mainly distributed in Kuandian Manchu Autonomous County (Liaoning Province, China); however, not much is known about the compounds (especially saponins) in Shizhu ginseng. Methods: A rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with MS/MS (UHPLC-MS/MS) method was developed to separate and identify saponins in Shizhu ginseng. Results: The separation was carried out on a Waters ACQUITY UPLC BEH $C_{18}$ column ($100mm{\times}2.1mm$, $1.7{\mu}m$) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase under a gradient elution at $40^{\circ}C$. The detection was performed on a Micromass Quattro Micro API mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 31 saponins were identified or tentatively characterized by comparing retention time and MS data with related literatures and reference substances. Conclusion: The developed UHPLC-MS/MS method was suitable for identifying and characterizing the chemical constituents in Shizhu ginseng, which provided a helpful chemical basis for further research on Shizhu ginseng.

Electrochemical spike oscillation st the Ni electrode interface (Ni 전극 계면에서 전기화학적 spike 발진)

  • 천장호;손광철;라극환
    • Journal of the Korean Institute of Telematics and Electronics A
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    • v.33A no.12
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    • pp.83-89
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    • 1996
  • The electrochemical spike oscillations at the nickel (Ni) electrode/(0.05M KHC$_{8}$H$_{4}$O$_{4}$) buffer solution (pH 9) interface have been studied using voltammetric and chronoamperometric methods. The nature of the periodic cathodic current spikes is the activation controlled currents due to the hydrogen evolution reaction and depends onthe fractioanl surface coverage of the adsorbed hydrogen intermediate or the cathodic potential. There is two kinds of the waveforms corresponding to two kinds of the cathodic current spike oscillations. The widths, periods, and amplitudes of the cathodic current spikes are 4 ms or 5ms, 151 ms or 302 ms, and < 30 mA or < 275 mA, respectively. The fast discharge and recombination reaction steps are 1.5 times and twice and faster than the slow discharge and recombination reaction steps. The fast and slow discharge and recombination reaction steps are 1.5 times and twice faster than the slow discharge and recombination reaction steps. The fast and slow discharge and recombination reactions corresponding to the fast and slow adsorption sites at the Ni cathode.

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Electrochemical Impulse Oscillations at the Platinum Group Electrode Interfaces (백금족 전력 계면에서 전기화학적 Impulse 발진)

  • 전장호;손광철;라극환
    • Journal of the Korean Institute of Telematics and Electronics A
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    • v.32A no.3
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    • pp.143-151
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    • 1995
  • The electrochemical impulse oscillations of the cathodic currents at the platinum group (Pt, Pd) electrode/(0.05M KHC$_{8}H_{4}O_{4}$) buffer solution interfaces have been studied using voltammetric, chronoamperometric, and electrochemical impedance methods. The periodic impulses of the cathodic currents are the activation controlled currents due to the hydrogen evolution reaction, and depend on the fractional surface coverage of the adsorbed hydrogen intermediate and potential. The oscillatory mechanism of the cathodic current impulses is connected with the unstable steady state of negative differential resistance. The widths and periods of the cathodic current impulses are 4ms or 5ms and 152.5ms or 305ms, respectively. The H$^{+}$ discharge reaction step is 38 or 61 times faster thatn the recombination reaction steps and the H$^{+}$ mass transport processes. The atom-atom recombination reaction step is twice faster thatn the atom-ion recombination reaction step. The two kinds of active sites corresponding to the atom-atom and atom-ion recombination reaction steps exist on the platinum group electrode surfaces.

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Determination of N. N-dimethylaniline in penicillins by GC-MS

  • Choi, Jung-Kap;Park, Man-Ki
    • Archives of Pharmacal Research
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    • v.4 no.2
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    • pp.85-90
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    • 1981
  • A quantitative GC-MS spectrometric assay was used for the determination of residual N, N-dimethylaniline as a contaminant in commercial penicillin derivatives from various sources. The assay utilizes selective ion focusing to monitor in a GC effluent the molecular ions of DMA generated by electron impact ionization. This method includes dissolution of the sample in alkaline solution, extraction of organic base with cyclohexane and injection into GC-MS with a 3% OV-17 column. Levels of 50 ppb of DMA were easily measured with a coeffecient of varation less than 5 % and recoveries from spiked samples exceeded 97 %. The results of the determinations of DMA in various commercial penicillins were relatively free of this contaminant.

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An Evaluation of Liquid Chromatography/Mass Specrometry with Atmospheric Pressure Chemical Ionizarion for the Rapid and Simultaneous Measurement of Carbamate Pesticides and Organophosphorus Pesticides

  • Kim, Byeong Ju;So, Hyeon Yeong
    • Bulletin of the Korean Chemical Society
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    • v.21 no.5
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    • pp.471-476
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    • 2000
  • Liquid chromatography/mass spectrometry with an atmospheric pressure chemical ionization interface (LC/APCI/MS) is evaluated for the simultaneous determination of carbamate pesticides and organophosphorus pesticides in a single chromatographic analysis. APCI mass spectra of those compounds were obtrained to study their ionization characteristics. APCI provided abundant ions such as protonated molecules and characteristic fragment ions for carbamate pesticides and organophosphorus pesticides. To evaluate the feasibility of the LC/APCI/MS for a routine quantitative analysis, the linearity and repeatability of LC/APCI/MS were examined by measuring standard solution mixtures of five carbamate pesticides and four organophosphorus pesticides over the range of 1 to 100 ㎍/mL. Teh peak areas in chromatograms of characteristic ions for those compounds showed less than 3% of variation from run to run. The standard calibration curves for the nine pesticides show good linearity in the concentration range. The detection limits of the LC/APCI/MS system for those compounds range from 0.006 to 0.2 ng.

EDUCATIONAL MANAGEMENT SCIENCE/OPERATIONS RESEARCH SOFTWARE: A SURVEY REVIEW

  • Kim, Eyong-B;Kang, Shin-Cheol
    • Journal of Korea Society of Industrial Information Systems
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    • v.5 no.2
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    • pp.70-77
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    • 2000
  • The purpose of this research was to investigate instructors perceptions on the use of quantitative educational software packages in management science and operations research (MS/OR) related courses. The investigation was conducted using a questionnaire survey of MS/OR instructors at US universities. The authors found that instructors were satisfied in the use of existing MS/OR educational software packages to effectively support their teaching in terms of computational speed, number of models offered, size of problems, and accuracy of algorithms. However, many instructors were not satisfied with the tutoring capability of packages such as 'what-if'analysis, graphics availability, explanation capacity, readability of output, and ease of use.

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Analysis of Alizarin Dye in Accelerated Degradation Conditions

  • Ahn, Cheunsoon
    • The International Journal of Costume Culture
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    • v.7 no.1
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    • pp.40-47
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    • 2004
  • The purpose of this research was to examine the degradation rate of alizarin in accelerated degradation conditions using the GC-MS quantitative analysis. Alizarin dye solution (2.5 x 10/sup -3/ M conc.) were kept in 150℃ oven for total of 7 days and the degradation rate was examined each day. 2.5 × 10/sup -4/M conc. alizarin dye solution was mixed with H₂O₂ according to [H₂O₂]/[dye] ratio 40 and were kept under 365㎚ UV for 2 hours, analyzed after 0, 30, 60, 90, 120min using the GC-MS. Gas chromatogram showed alizarin peak at 9.96 - 10.13 min. retention time range and residual peaks in the wide range from 9.6 to 11.1 min. Oven degradation exhibited an initial decrease in the amount of alizarin, which was followed by increasing amount in 4/sup th/ day. The decrease in the alizarin was significantly shown by the 7/sup th/ day. Same pattern was also observed in the H₂O₂/UV/O₂ degradation samples and was verified ed by the UV-VIS spectra. The differences in the amount of alizarin between 1/sup st/ day and 4/sup th/ day samples, 4/sup th/ day and 7/sup th/ day samples, and Control and 7/sup th/ day samples of the oven degradation were significant at alpha .20.

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Analysis of Heterocyclic Amines in Mainstream Cigarette Smoke using by LC-MS/MS (LC-MS/MS를 이용한 담배 연기 중 Heterocyclic Amines의 분석)

  • Kim, Ick-Joong;Jang, Gi-Chul;Ji, Sang-Un;Min, Hye-Jeong;Kim, Hyo-Keun;Hwang, Geon-Jung
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.1
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    • pp.33-38
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    • 2008
  • This study was carried out to determine the analytical methods for heterocyclic amines(HAs) of the tobacco smoke by LC/MS/MS. HAs have been found in pyrolysate of protein and cooked food including protein, were known the Sugimura compound. HAs content of the smoke were known to exist very low ppb level. Especially, some of HAs are mutagenic and carcinogenic compounds. In according to IARC, the toxicity of N-heterocyclic amines classified IARC class 2A or 2B group. Precursors of these compounds are glutamic acid, protein and free amino acids including tryptophan, therefore, the precursors have been proved in cooked food continuously. This study was investigate multiple analysis methods for HAs and HAs contents of some commercial products. In this study, we used the linear type smoking machine for HAs analysis. At the ISO conditions, mainstream smoke was collected on cambridge filter pad, and then cambridge filter pad was extracted by 0.1% acetic acid. The extracted solution were passed cation exchange SPE cartridge to remove matrix, samples were analyzed using LC/MS/MS on MRM mode. From the result that optimized this methods, the correlation coefficient(R) of the individual compounds were good linearity over 0.999, recovery rate over 96% and the limit of detection were good values between 0.06 to 0.37 ng/mL, In addition, HAs content of some commercial products were in range of 0.02 to 43.8 ng/cig.

Determination of 8-iso-PGF as Oxidative Stress Marker in Human Urine by High Performance Liquid Chromatography with Tandem Mass Spectrometry (LC/MS/MS를 이용한 산화성 스트레스 지표로써 소변 중 8-iso-PGF 분석)

  • Kho, Young-Lim;Lee, Eun-Hee;Chae, Hong-Jae;Choi, Kyung-Ho;Paik, Do-Myung
    • Journal of Environmental Health Sciences
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    • v.36 no.1
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    • pp.44-51
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    • 2010
  • This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.

Verification of Analytical Method of Azaspiracid Toxins in Shellfish and Tunicates by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)를 이용한 패류 및 피낭류 중 아자스필산 분석법의 유효성 검증)

  • Cho, Sung Rae;Jeong, Sang Hyeon;Park, Kunbawui;Yoon, Minchul;Kim, Dong Wook;Son, Kwang Tae;Ha, Kwang Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.54 no.4
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    • pp.404-410
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    • 2021
  • Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R2) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 ㎍/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 ㎍/kg and 0.23-0.50 ㎍/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.