• Title/Summary/Keyword: Positive Column

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Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot-Liquid Chromatography-Mass Spectrometry

  • Jang, Haejong;Mai, Xuan-Lan;Lee, Gunhee;Ahn, Jae Hyoung;Rhee, Jongsook;Truong, Quoc-Ky;Vinh, Dinh;Hong, Jongki;Kim, Kyeong Ho
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.95-99
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    • 2018
  • An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.

A Sensitive and Rapid LC-MS/MS Method for Determination of Berberine in Human Plasma

  • Kim, Jae Hee;Mai, Xuan-Lan;Kim, Kyu Yeon;Sim, Min-Seok;Lee, So-Yeon;Seo, Hee-Won;Lee, Gunhee;Kim, Dae-Jung;Kim, Kyeong Ho
    • Mass Spectrometry Letters
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    • v.10 no.2
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    • pp.56-60
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    • 2019
  • Coptidis Rhizoma (CR) has been used widely in traditional medicine to treat common diseases. This study aimed to develop a high-sensitivity liquid chromatography-tandem mass (LC-MS) spectrometry method for the evaluation of the pharmacokinetics of a new natural product that contain CR extract with the main bioactive compound, berberine, at trace concentrations. Human plasma samples were pretreated with methanol by a protein precipitation method. Berberine was analyzed on a Kinetex C18 column ($2.1mm{\times}50mm$, $100{\AA}$, $1.7{\mu}m$) using a mobile phase of 10 mM ammonium formate/0.1% formic acid in water (A) and acetonitrile (B) (50:50, v/v) with a flow rate of 0.25 mL/min. The analyte was detected by using electrospray ionization in positive mode with multiple reaction monitoring (MRM). The method was sensitive, with a lower limit of quantification of 1 pg/mL, which has not been previously obtained. The method was validated (over the range of 1-50 pg/mL) and applied successfully for the pharmacokinetic study of human plasma samples.

Inhibitory effect of Fucofuroeckol-A from Eisenia bicyclis on tyrosinase activity and melanin biosynthesis in murine melanoma B16F10 cells

  • Shim, Kil Bo;Yoon, Na Young
    • Fisheries and Aquatic Sciences
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    • v.21 no.11
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    • pp.35.1-35.7
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    • 2018
  • Background: The aim of this study was to investigate the in vitro inhibitory effects of Fucofuroeckol-A isolated from Eisenia bicyclis against tyrosinase activity and 3-isobutyl-1-methylxanthine (IBMX)-induced melanin biosynthesis in B16F10 melanoma cells. Result: Among the ethanolic (EtOH) extract of E. bicyclis and its organic solvent fractions, the ethyl acetate (EtOAc) soluble fraction showed a noticeable inhibitory effect on mushroom tyrosinase with an $IC_{50}$ value of $37.6{\pm}0.1{\mu}g/mL$. Repeated column chromatography of the active EtOAc fraction resulted in the isolation of Fucofuroeckol-A. It evidenced more potent tyrosinase inhibitory effect with an $IC_{50}$ value of $11.4{\pm}1.4{\mu}M$ than arbutin ($IC_{50}=1076.6{\pm}44.3{\mu}M$), which was used as a positive control. Lineweaver-Burk plots suggest that Fucofuroeckol-A plays as a noncompetitive inhibitor against tyrosinase. Furthermore, we have evaluated the inhibitory effects of Fucofuroeckol-A on IBMX-induced melanin formation in B16F10 melanoma cells. Fucofuroeckol-A ($12.5-100{\mu}M$) exhibited a significant inhibition of melanin production in the melanoma cells. Conclusion: In the present study, we suggested that Fucofuroeckol-A might prove possibility as a novel inhibitor of melanin biosynthesis in cosmetic applications.

Hierarchical neural network for damage detection using modal parameters

  • Chang, Minwoo;Kim, Jae Kwan;Lee, Joonhyeok
    • Structural Engineering and Mechanics
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    • v.70 no.4
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    • pp.457-466
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    • 2019
  • This study develops a damage detection method based on neural networks. The performance of the method is numerically and experimentally verified using a three-story shear building model. The framework is mainly composed of two hierarchical stages to identify damage location and extent using artificial neural network (ANN). The normalized damage signature index, that is a normalized ratio of the changes in the natural frequency and mode shape caused by the damage, is used to identify the damage location. The modal parameters extracted from the numerically developed structure for multiple damage scenarios are used to train the ANN. The positive alarm from the first stage of damage detection activates the second stage of ANN to assess the damage extent. The difference in mode shape vectors between the intact and damaged structures is used to determine the extent of the related damage. The entire procedure is verified using laboratory experiments. The damage is artificially modeled by replacing the column element with a narrow section, and a stochastic subspace identification method is used to identify the modal parameters. The results verify that the proposed method can accurately detect the damage location and extent.

Screening of Nitrosamine Impurities in Sartan Pharmaceuticals by GC-MS/MS

  • Chang, Shu-Han;Ho, Hui-Yu;Zang, Chi-Zong;Hsu, Ya-Hui;Lin, Mei-Chih;Tseng, Su-Hsiang;Wang, Der-Yuan
    • Mass Spectrometry Letters
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    • v.12 no.2
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    • pp.31-40
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    • 2021
  • Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

Simultaneous Liquid Chromatography Tandem Mass Spectrometric Determination of 35 Prohibited Substances in Equine Plasma for Doping Control

  • Kwak, Young Beom;Yu, Jundong;Yoo, Hye Hyun
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.158-165
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    • 2022
  • Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

The Effect of Vertical Strut in Circular Arch Lattice Structure by Selective Laser Sintering for Lightweight Structure

  • Sangwon Lee;Jae-An Jeon;Sang-Eui Lee
    • Composites Research
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    • v.36 no.3
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    • pp.173-179
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    • 2023
  • The sandwich structure, consisting of a core and a face sheet, is used for lightweight structural application. Generally, cellular structures like honeycomb, foam, and lattice structures are utilized for the core. Among these, lattice structures have several advantages over other types of structures. In other studies, curved lattice structures were reported to have higher mechanical properties than straight structures by converting shear stresses acting on the structure into compressive stresses. Moreover, the addition of vertical struts can have a positive effect on the mechanical properties of the lattice structure. For the purpose, two lattice structures with Circle Arch (CC) and Circular Arch with a vertical column (CC_C) were studied, which were fabricated by using selective laser sintering was conducted. The result showed that CC_C has dramatic performance improvements in specific strength, modulus, and strain energy density compared to CC, confirming that vertical struts played a significant role in the lattice core. Finite element analysis was employed to determine the cause of the stress behavior of CC and CC_C. This study is expected to help design structurally superior lattice cores and sandwich structures.

Experimental investigation of local stress distribution along the cross-section of composite steel beams near joints

  • Sangwook Park;Patricia Clayton;Todd A. Helwig;Michael D. Engelhardt;Eric B. Williamson
    • Steel and Composite Structures
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    • v.51 no.5
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    • pp.563-573
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    • 2024
  • This research experimentally evaluated the local stress distribution along the cross-section of composite beams under both positive and negative moments. The experiment utilized a large-scale, two-story, two-by-three bay steel gravity frame with a concrete on metal deck floor system. The composite shear connections, which are nominally assumed to be pinned under gravity loading, can develop non-negligible moment-resisting capacity when subjected to lateral loads. This paper discusses the local stress distribution, orshear lag effects, observed near the beam-to-column connections when subjected to combined gravity and lateral loading. Strain gauges were used for measurements along the beam depth at varying distances from the connection. The experimental data showed amplified shear lag effects near the unconnected region of the beam web and bottom flange under the applied loading conditions. These results indicate that strain does not vary linearly across the beam cross-section adjacent to the connection components. This insight has implications for the use of experimental strain gauge data in estimating beam demands near the connections. These findings can be beneficial in informing instrumentation plans for future experimental studies on composite beams.

System-level performance of earthquake-damaged concrete bridges with repaired columns

  • Giacomo Fraioli;Yu Tang;Yang Yang;Lesley H. Sneed
    • Computers and Concrete
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    • v.33 no.4
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    • pp.361-372
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    • 2024
  • Reinforced concrete (RC) bridge columns are typically designated as the primary source of energy dissipation for a bridge structure during an earthquake. Therefore, seismic repair of RC bridge columns has been studied extensively during the past several decades. On the other hand, few studies have been conducted to evaluate how repaired column members influence the system-level response of an RC bridge structure in subsequent earthquakes. In this study, a numerical model was established to simulate the response of two large-scale RC columns, repaired using different techniques, reported in the literature. The columns were implemented into a prototype bridge model that was subjected to earthquake loading. Incremental dynamic analysis (IDA) and fragility analysis were conducted on numerical bridge models to evaluate the efficacy of the repairs and the post-repair seismic performance of the prototype bridge that included one or more repaired columns in various locations. For the prototype bridge herein modeled, the results showed that a confinement-enhanced oriented repair would not affect the seismic behavior of the prototype bridge. Increasing the strength of the longitudinal reinforcement could effectively reduce the drift of the prototype bridge in subsequent earthquakes. A full repair configuration for the columns was the most effective method for enhancing the seismic performance of the prototype bridge. To obtain a positive effect on seismic performance, a minimum of two repaired columns was required.

Integrative Korean Medicine Treatment for Low Back Pain with Butterfly Vertebra: Two Clinical Cases

  • Dong-Hwan Lee;Oh-Bin Kwon;Jae-Young Lee;Hyo-Rim Kim;Tae-Jun Lee;Sung-Hwan Cho;Kang-Moo Goo;Ja-Yean Son;Seok-Gyu Yang;Yu-Ra Im
    • Journal of Acupuncture Research
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    • v.41
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    • pp.168-175
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    • 2024
  • The butterfly vertebra is a rare congenital anomaly of the spine, which arises from an asymmetric fusion defect in the embryonic vertebral column. This report delineates an integrative Korean medicine treatment administered to two patients who presented with low back pain associated with asymptomatic butterfly vertebrae. The patients received comprehensive treatment comprising acupuncture, Chuna therapy, pharmacopuncture, herbal medicine, and cupping therapy. The efficacy of the treatments was assessed utilizing diverse parameters, including a numerical rating scale, range of motion of the lumbar spine, Oswestry Disability Index, EuroQoL 5-Dimension 5-Level, and patient global impression of change. After the treatment, a notable improvement was noted in the evaluated indicators. These positive outcomes suggest that integrative Korean medicine treatment is suitable for patients experiencing low back pain associated with asymptomatic butterfly vertebrae.