• Title/Summary/Keyword: Particle Size Response

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Qualitative and quantitative assessment of process related impurities in Brigatinib raw material and formulations using HPLC

  • Attada Tharun;Potnuru Jagadeesh;B Srinivasa Kumar;Kota Thirumala Prasad;Venkateswara Rao Anna
    • Analytical Science and Technology
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    • v.36 no.4
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    • pp.180-190
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    • 2023
  • The presence of process related impurities in any drug or the drug product was associated with its safety, stability and efficacy. The overall literature survey proved that there is no method published on the assessment of process related impurities in brigatinib. In this study, a simple, reliable and stable HPLC qualitative method was reported for quantification of process related impurities with easy and quick extraction procedure. The impurities along with standard brigatinib was resolved on Lichrospher® C18 (250 mm × 4.6 mm; 5 ㎛ particle size) column in room temperature using methanol, acetonitrile, pH 4.5 phosphate buffer in 55:25:20 (v/v) at 1.0 mL/min as mobile phase and UV detection at 261 nm. The method produces well resolved peaks at retention time of 4.60 min, 12.28 min, 3.37 min, 7.34 min and 8.39 min respectively for brigatinib, impurity A, B, C and D. The method produces a very sensitive detection limit of 0.0065 ㎍/mL, 0.0068 ㎍/mL, 0.0053 ㎍/mL and 0.0058 ㎍/mL for impurity A, B, C and D respectively with calibration curve linear in the concentration range of 22.5-135 ㎍/mL for brigatinib and 0.0225-0.135 ㎍/mL for impurities. The method produces all the validation parameters under the acceptable level and doesn't produces any considerable changes in peak area response while minor changes in the developed method conditions. The method can effectively resolve the unknown stress degradation products along with known impurities with less % degradation. The method can efficiently resolve and quantify the impurities in formulation and hence can suitable for the routine quality analysis of brigatinib in raw material and formulation.

Immunization of mice with chimeric protein-loaded aluminum hydroxide and selenium nanoparticles induces reduction of Brucella melitensis infection in mice

  • Tahereh Goudarzi;Morteza Abkar;Zahra Zamanzadeh;Mahdi Fasihi-Ramandi
    • Clinical and Experimental Vaccine Research
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    • v.12 no.4
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    • pp.304-312
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    • 2023
  • Purpose: Due to the many problems with commercially available vaccines, the production of effective vaccines against brucellosis is a necessity. The aim of this study was to evaluate the immune responses caused by the chimeric protein consisting of trigger factor, Bp26, and Omp31 (TBO) along with aluminum hydroxide (AH/TBO) and selenium (Se/TBO) nanoparticles (NPs) as adjuvants in mouse model. Materials and Methods: Recombinant antigen expression was induced in Escherichia coli BL21 (DE3) bacteria using IPTG (isopropyl-d-1-thiogalactopyranoside). Purification and characterization of recombinant protein was conducted through NiFe3O4 NPs, sodium dodecyl sulfate-polyacrylamide gel electrophoresis, and Western blot. NP characteristics, including morphology and particle size, were measured in vitro. The recombinant TBO was loaded on to AH and Se NPs and were administered subcutaneously. After mice immunization, measurement of antibody titter and protection assay was performed. Results: The average sizes of AH and Se NPs were about 60 nm and 150 nm, respectively. The enzyme-linked immunosorbent assay results showed that the serum of mice immunized by subcutaneous injection with both nanovaccines produced significant immunoglobulin G (IgG) responses against the chimeric antigen. The results of TBO-specific IgG isotype (IgG2a/IgG1) analysis showed that both AH and Se NPs induced a type to T-helper immune response. In addition, the results of the challenge with the pathogenic strain of Brucella melitensis 16M showed that vaccinated mice with AH/TBO NPs indicated a higher reduction of bacterial culture than immunized mice with Se/TBO NPs and TBO alone. Conclusion: The results showed that AH NPs carrying chimeric antigen can be a promising vaccine candidate against brucellosis by producing protective immunity.

Physio-mechanical and X-ray CT characterization of bentonite as sealing material in geological radioactive waste disposal

  • Melvin B. Diaz;Sang Seob Kim;Gyung Won Lee;Kwang Yeom Kim;Changsoo Lee;Jin-Seop Kim;Minseop Kim
    • Geomechanics and Engineering
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    • v.34 no.4
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    • pp.449-459
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    • 2023
  • The design and development of underground nuclear waste repositories should cover the performance evaluation of the different components such as the construction materials because the long term stability will depend on their response to the surrounding conditions. In South Korea, Gyeonju bentonite has been proposed as a candidate to be used as buffer and backfilling material, especially in the form of blocks to speed up the construction process. In this study, various cylindrical samples were prepared with different dry density and water content, and their physical and mechanical properties were analyzed and correlated with X-ray CT observations. The main objective was to characterize the samples and establish correlations for non-destructive estimation of physical and mechanical properties through the utilization of X-ray CT images. The results showed that the Uniaxial Compression Strength and the P-wave velocity have an increasing relationship with the dry density. Also, a higher water content increased the values of the measure parameters, especially for the P-wave velocity. The X-ray CT analysis indicated a clear relation between the mean CT value and the dry density, Uniaxial Compression Strength, and P-wave velocity. The effect of the higher water content was also captured by the mean CT value. Also, the relationship between the mean CT value and the dry density was used to plot CT dry densities using CT images only. Moreover, the histograms also provided information about the samples heterogeneity through the histograms' full width at half maximum values. Finally, the particle size and heterogeneity were also analyzed using the Madogram function. This function identified small particles in uniform samples and large particles in some samples as a result of poor mixing during preparation. Also, the μmax value correlated with the heterogeneity, and higher values represented samples with larger ranges of CT values or particle densities. These image-based tools have been shown to be useful on the non-destructive characterization of bentonite samples, and the establishment of correlations to obtain physical and mechanical parameters solely from CT images.

Intracellular Signaling Pathway for Host Defense Mechanisms against Piscine Nervous Necrosis Virus (NNV) (어류신경괴사증바이러스(nervous necrosis virus, NNV) 감염에 따른 숙주의 방어기전관련 세포신호전달)

  • Kim, Jong-Oh
    • Journal of Life Science
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    • v.30 no.4
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    • pp.402-409
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    • 2020
  • Nervous necrosis virus (NNV) contains a bi-segmented viral genome, RNA1 (3.4 kb, RdRp), and RNA2 (1.4 kb, capsid protein) in a small particle (25 nm). Despite its extremely compact size, NNV has caused serious damage by infecting approximately 120 fish species worldwide since it was first reported in the late 1980s. In order to minimize the damage caused by NNV infection and develop effective vaccines, it is necessary to understand the intra cellular signaling system according to NNV infection. NNV infection induces cell cycle arrest at the G1 phase via the p53-dependent pathway to use the cellular system for its replication. Otherwise, host cells recognize NNV infection through the RIG-1-like receptor (RLR) signaling pathway to control the virus and infected cells, and then ISGs required for antiviral action are activated via the IFN signaling pathway. Moreover, apoptosis of infected cells is triggered by the unfolded protein response (UPR) through ER stress and mitochondria-mediated cell death. Cell signaling studies on the NNV infection mechanisms are still at an early stage and many pathways have yet to be identified. Understanding the various disease-specific cellular signaling systems associated with NNV infection is essential for rapid and accurate diagnosis and vaccine development.

Propagation characteristics of blast-induced vibration to fractured zone (파쇄영역에 따른 발파진동 전파특성)

  • Ahn, Jae-Kwang;Park, Duhee;Park, Ki-Chun;Yoon, Ji Nam
    • Journal of Korean Tunnelling and Underground Space Association
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    • v.19 no.6
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    • pp.959-972
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    • 2017
  • In evaluation of blast-induced vibration, peak particle velocity (PPV) is generally calculated by using attenuation relation curve. Calculated velocity is compared with the value in legal requirements or the standards to determine the stability. Attenuation relation curve varies depending on frequency of test blasting, geological structure of the site and blasting condition, so it is difficult to predict accurately using such an equation. Since PPV is response value from the ground, direct evaluation of the structure is impractical. Because of such a limit, engineers tend to use the commercial numerical analysis program in evaluating the stability of the structure more accurately. However, when simulate the explosion process using existing numerical analysis program, it's never easy to accurately simulate the complex conditions (fracture, crushing, cracks and plastic deformation) around blasting hole. For simulating such a process, the range for modelling will be limited due to the maximum node count and it requires extended calculation time as well. Thus, this study is intended to simulate the elastic energy after fractured zone only, instead of simulating the complex conditions of the rock that results from the blast, and the analysis of response characteristics of the velocity depending on shape and size of the fractured zone was conducted. As a result, difference in velocity and attenuation character were calculated depending on fractured zone around the blast source appeared. Propagation of vibration tended to spread spherically as it is distanced farther from the blast source.

Gas Sensing Behaviors of SnO2:Cu Nanostructures for CH4, CH3CH2CH3 Gas (SnO2:Cu 나노 구조물의 CH4, CH3CH2CH3 가스 감응 특성)

  • Lee, Ji-Young;Yu, Yoon-Sic;Yu, Il
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.12
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    • pp.974-978
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    • 2012
  • The effect of Cu coating on the sensing properties of nano $SnO_2:Cu$ based sensors for the $CH_4$, $CH_3CH_2CH_3$ gas was studied. This work was focussed on investigating the change of sensitivity of nano $SnO_2:Cu$ based sensors for $CH_4$, $CH_3CH_2CH_3$ gas by Cu coating. Nano sized $SnO_2$ powders were prepared by solution reduction method using stannous chloride($SnCl_2{\cdot}2H_2O$), hydrazine($N_2H_2$) and NaOH and subsequent heat treatment. XRD patterns showed that nano $SnO_2$ powders with rutile structure were grown with (110), (101), (211) dominant peak. The particle size of nano $SnO_2:Cu$ powders at 8 wt% Cu was about 50 nm. $SnO_2$ particles were found to contain many pores, according to SEM analysis. The sensitivity of nano $SnO_2:Cu$ based sensors was measured for 5 ppm $CH_4$ gas and $CH_3CH_2CH_3$ gas at room temperature by comparing the resistance in air with that in target gases. The sensitivity for both $CH_4$ and $CH_3CH_2CH_3$ gases was improved by Cu coating on the nano $SnO_2$ surface. The response time and recovery time of the $SnO_2:Cu$ gas sensors for the $CH_4$ and $CH_3CH_2CH_3$ gases were 18~20 seconds, and 13~15 seconds, respectively.

A Literature Review on Nano-Modified Implant Surfaces (나노구조 표면에 관한 문헌고찰)

  • Park, Go-Woon;Cha, Min-Sang;Kim, Dae-Gon;Park, Chan-Jin;Cho, Lee-Ra
    • Journal of Dental Rehabilitation and Applied Science
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    • v.29 no.2
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    • pp.141-151
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    • 2013
  • The nano-surface modification techniques could be classified; internal modifications which enhance surface roughness and porosity in nano level and external modifications as nano particle coating. Nano-modified implant surface has various morphograpies such as nanotube, nanopit, nanonodule and polymorphic structures. Creating surface depends upon preparation method and material, however, there is no standard preparation technique not yet. The nano-modified surfacet is electrochemically stable comparing with the surface modified in micron level. Nano-modified surface has little cytotoxicity, stimulates osteoblast proliferation and differentiation. Moreover, it decreases soft tissue intervention by interrupting the proliferation of fibroblast. Nanostructure has similar size and shape with cells and proteins, consequently leads to good biocompatibility and enhanced osseointegration. However, the actual effect in vivo is limited, due to the distance of effect. Even if nano-modified surface has antibiotic property due to photocatalysis, short duration time makes clinical application questionable. Further investigations should focus on the optimal nano-modified surface, which has many potentials.

Evaluation of Field Application and Estimation of Bedload Discharge in the Forest Watershed using the Hydrophone (하이드로폰을 이용한 산림유역 소류사 유출량 산정 및 현장 적용성 검토)

  • Seo, Jun-Pyo;Kim, Ki-Dae;Woo, Choong-Shik;Lee, Chang-Woo;Lee, Heon-Ho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.12
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    • pp.807-818
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    • 2020
  • In this study, hydrophones using acoustic sensors were used to estimate the amount of bedload discharge in a forested watershed. The reaction characteristics were analyzed through hydrophone flume tests and field tests, and the quantitative bedload discharge was calculated and compared with that measured by a pit sampler. The hydrophone reaction changed the pulse according to the flow rate change, but did not react to standard sand. The pulse was different depending on the particle size and weight, and accordingly, there was a specific channel showing a suitable response. For a hydrophone installed in the field, by using an automatic impact device, the reaction characteristics of each channel were analyzed to confirm normal operation of the sensor and the suitability of the output value of each channel. In addition, a suitable channel was selected for the estimation of bedload discharge. The bedload discharge formula was developed using a hydrophone pulse and the average flow rate, and was compared with the measured data in the pit sampler in the study site. As a result of the study, if a hydrophone is used for monitoring the bedload in forested watersheds, it is considered effective in quantitatively estimating the weight of bedload discharge.

Characteristics of Glycyrrhiza uralensis extract-loaded chitosan nanocapsules and their antioxidant activity (감초 추출물 함유 키토산 나노캡슐의 특성 및 항산화 활성)

  • Kim, Min Jung;Lee, Ji-Soo;Lee, Hyeon Gyu
    • Korean Journal of Food Science and Technology
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    • v.53 no.4
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    • pp.479-485
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    • 2021
  • To improve the oxidative stability of Glycyrrhiza uralensis extract (GU), GU extraction conditions were optimized for maximal antioxidant activity, and GU-loaded nanocapsules were prepared by chitosan ionic gelation. The optimized ethanol concentration and extraction time were 83.0% and 32.6 min, respectively, using response surface methodology. The particle size of the GU-loaded nanocapsules ranged from 280 to 370 nm. A GU extract of 0.8 mg/mL and chitosan concentration of 2.0 mg/mL were selected as the optimal conditions for entrapment and loading efficiency. Both free GU and GU-loaded chitosan nanocapsules exhibited concentration-dependent antioxidant activity. However, the antioxidant protection factor of GU was effectively maintained when it was entrapped within the chitosan nanocapsules. In conclusion, chitosan nanoencapsulation is a potentially valuable technique for improving the oxidative stability of GU.