• 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.

• Analytical Science and Technology
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• v.37 no.1
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• pp.25-38
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• 2024

The study aimed to investigate a novel approach by utilizing liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) to separate, identify and characterize very nominal quantities of degradation products (DPs) of balsalazide along with its process related impurities without isolation from their reaction mixtures. The impurities along with balsalazide were resolved on spherisorb ODS2 (250×4.6 mm, 5.0 ㎛) column at room temperature using 0.2 M sodium acetate solution at pH 4.5 and methanol in the ratio of 55:45 (v/v) as mobile phase pumped isocratically at 1.0 mL/min as mobile phase and UV detection at 255 nm. The method shows sensitive detection limit of 0.003 ㎍/mL, 0.015 ㎍/mL and 0.009 ㎍/mL respectively for impurity 1, 2 and 3 with calibration curve liner in the range of 50-300 ㎍/mL for balsalazide and 0.05-0.30 for its impurities. The balsalazide pure compound was subjected to stress studies and a total of four degradation products (DPs) were formed during the stress study and all the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon LC-MS/MS. The DPs were identified as 3-({4-[(E)-(4-hydroxyphenyl) diazenyl]benzoyl}amino)propanoic acid (DP 1), 4-[(E)-(4-hydroxyphenyl)diazenyl] benzamide (DP 2), 5-[(E)-(4-carbamoylphenyl)diazenyl]-2-hydroxybenzoic acid (DP 3) and 3-({4-[(E)-phenyldiazenyl]benzoyl}amino)propanoic acid (DP 4). Based on findings, it was concluded that, the proposed method was successfully applicable for routine analysis of balsalazide and its process related impurities in pure drug and formulations and also applicable for identification of known and unknown impurities of balsalazide.

• Analytical Science and Technology
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• v.20 no.2
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• pp.131-137
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• 2007

The urania-gadolinia fuels were dissolved with nitric acid. The analytical conditions of ICP-AES for the direct determinations of gadolinium in the uranium matrices without separation process were investigated. Based on the effect of uranium on gadolinium intensity, the best wavelength for gadolinium was 336.223 nm. The relative deviation of two methods, direct and indirect measurements with anion exchange chromatography, was less than 5 %. Therefore it was possible for this procedure directly to measure 5~10 wt.% of gadolinium in urania-gadolinia fuels without separation by ICP-AES.

• Analytical Science and Technology
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• v.16 no.3
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• pp.218-225
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• 2003

Hydrogen Chloride is among the most problematic gases used in semiconductor process. It raises serious environmental and health problems due to its extreme toxicity. This study is to develop a method to effectively remove hydrogen chloride gas during the process by using various types of inorganic gas adsorption agents, which have not been attempted in the conventional methods. The removal efficiency of the gas was both qualitatively and quantitatively measured by a FT-IR spectrophotometer. The whole device for the measurement has been designed and built in our lab. The removal efficiencies of hydrogen chloride gas were compared between those tested resins; zeolite A, modified AgA zeolite, ZnO, and $AgMnO_3$. The experimental result revealed that ZnO showed the best efficiency that had removed 0.067 g of HCl per 1 g of the resin used.

• Membrane and Water Treatment
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• v.7 no.2
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• pp.87-100
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• 2016

A numerical simulation of membrane evaporation process was carried out in this work. The aim of simulation is to describe transport of water through porous membranes applicable to the concentration of aqueous solutions. A three-dimensional mathematical model was developed which considers transport phenomena including mass, heat, and momentum transfer in membrane evaporation process. The equations of model were then solved numerically using finite element method. The results of simulation in terms of evaporation flux were compared with experimental data, and confirmed the accuracy of model. Moreover, profile of pressure, concentration, and heat flux were obtained and analyzed. The results revealed that developed 3D model is capable of predicting performance of membrane evaporators in concentration of aqueous solutions.

• Advances in environmental research
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• v.2 no.3
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• pp.179-202
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• 2013

Bisphenol A and other alkylphenols are widely used in plastic and other industrial consumer products. Release of these compounds into the aquatic environment during their manufacture, use and disposal has been a great scientific and public concern due to their toxicity at high concentrations and endocrine disrupting effects at low concentration on aquatic wildlife and human beings. This paper reviews the published data and researches on the environmental occurrence, distribution, health effects and analytical techniques of bisphenol A and alkylphenols. The aim is to provide an overview of the current understanding about bisphenol A and alkylphenols in the environment and the difficulties faced today in order to establish standard and systematic environmental analysis and assessment process for these endocrine disruptor compounds.

• Analytical Science and Technology
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• v.12 no.6
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• pp.465-471
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• 1999

Chloromethylated polystyrene resins supported diethylenetriamine of linear and claw types have been prepared by the reaction of diethylenetriamine with chloromethylated polystyrene. The kinetics of adsorption of transition metal ions on polystyrene resins were measured by the limited-bath technique. This paper reports the results of the diffusion coefficients, entropies of activation, and free energies of activation. The ratedetermining step of the adsorption of transition metals on the resins is a process of diffusion through the particles.

• Analytical Science and Technology
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• v.32 no.3
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• pp.77-87
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• 2019

High viscosity carbon black dispersions are used in various industrial fields such as color cosmetics, rubber, tire, plastic and color filter ink. However, carbon black particles are unstable to heat due to inherent characteristics, and it is very difficult to keep the quality of the product constant due to agglomeration of particles. In general, particle size analysis is performed by dynamic light scattering (DLS) during the dispersion process in order to select the optimum dispersant in the carbon black dispersion process. However, the existing low viscosity analysis provides reproducible particle distribution analysis results, but it is difficult to select the optimum dispersant because it is difficult to analyze the reproducible particle distribution at high viscosity. In this study, dynamic light scattering (DLS) and asymmetrical flow field-flow fractionation (AsFlFFF) analysis methods were compared for reproducible particle size analysis of high viscosity carbon black. First, the stability of carbon black dispersion was investigated by particle size analysis by DLS and AsFlFFF according to milling time, and the validity of analytical method for the selection of the optimum dispersant useful for carbon black dispersion was confirmed. The correlation between color and particle size of particles in high viscosity carbon black dispersion was investigated by using colorimeter. The particle size distribution from AsFlFFF was consistent with the colorimetric results. As a result, the correlation between AsFlFFF and colorimetric results confirmed the possibility of a strong analytical method for determining the appropriate dispersant and milling time in high viscosity carbon black dispersions. In addition, for nanoparticles with relatively broad particle size distributions such as carbon black, AsFlFFF has been found to provide a more accurate particle size distribution than DLS. This is because AsFlFFF, unlike DLS, can analyze each fraction by separating particles by size.

• Korean Journal of Clinical Laboratory Science
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• v.38 no.2
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• pp.117-124
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• 2006

The analytical measurement range (AMR) is the range of analyte values that a method can directly measure on a specimen without any dilution, concentration, or other pretreatment not part of the usual assay process. The linearity of the AMR is its ability to obtain test results which are directly proportional to the concentration of analyte in the sample from the upper and lower limit of the AMR. The AMR validation is the process of confirming that the assay system will correctly recover the concentration or activity of the analyte over the AMR. The test specimen must have analyte values which, at a minimum, are near the low, midpoint, and high values of the AMR. The AMR must be revalidated at least every six months, at changes in major system components, and when a complete change in reagents for a procesure is introduced; unless the laboratory can demonstrate that changing the reagent lot number does not affect the range used to report patient test results. The AMR linearity was total protein (0-16.6), albumin (0-8.1), total bilirubin (0-18.1), alkaline phosphatase (0-1244.3), aspartate aminotransferase (0-1527.9), alanine aminotransferase (0-1107.9), gamma glutamyl transpeptidase (0-1527.7), creatine kinase (0-1666.6), lactate dehydrogenase (0-1342), high density lipoprotein cholesterol (0.3-154.3), sodium (35.4-309), creatinine (0-19.2), blood urea nitrogen (0.5-206.2), uric acid (0-23.9), total cholesterol (-0.3-510), triglycerides (0.7-539.6), glucose (0-672.7), amylase (0-1595.3), calcium (0-23.9), inorganic phosphorus (0.03-17.0), potassium (0.1-116.5), chloride (3.3-278.7). We are sure that materials for the AMR affect the evaluation of the upper limit of the AMR in the process system.

• Journal of Industrial and Engineering Chemistry
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• v.68
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• pp.42-47
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• 2018

This work reports a facile and effective antibacterial coating for oxide substrates. As a coating material, a random copolymer, abbreviated as poly(TMSMA-r-PEGMA), was synthesized by radical polymerization of 3-(trimethoxysilyl)propyl methacrylate (TMSMA) and poly(ethylene glycol) methyl ether methacrylate (PEGMA). Polymeric self-assembled monolayers of poly(TMSMA-r-PEGMA) were formed on various inorganic oxide substrates, including silicon oxide, titanium dioxide, aluminum oxide, and glass, via the simple dip-coating process. The polymer-coated substrates were characterized by ellipsometry, contact angle measurements, and X-ray photoelectron spectroscopy. The bacterial adhesion on the polymer-coated substrates was completely suppressed compared to that on the uncoated substrates.