• Korean Journal of Veterinary Service
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• v.43 no.4
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• pp.261-265
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• 2020

Each commercial cyromazine insecticide has different HPLC conditions. The aim of this study was to establish a standardized chromatographic method for the determination of cyromazine in commercial insecticides. The separation was achieved on two C18 columns - Waters® Bondapak C (4×300 nm i.d., 10 ㎛) and X bridge (4.6×250 nm i.d., 5 ㎛) using a mobile phase composed of water/methanol/ethanolamine (76:24:0.1, v/v), with UV detection at wavelengths 230 nm and 254 nm. A total of six commercial cyromazine insecticides were analyzed. In this study, the optimal high-performance liquid chromatography conditions for the analysis of cyromazine were as follows: a mobile phase of water/methanol/ethanolamine (76:24:0.1, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm using a X bridge C18 column (4.6×250 nm i.d., 5 ㎛) at a column temperature of 25℃. The calibration curve was linear in the concentration range of 5~50 ㎍/mL, with a correlation coefficient of 0.99995. The cyromazine detection limit was 0.2 ㎍/mL, and the limit of quantification was 0.59 ㎍/mL. The percentage recovery ranged from 99.8% to 101.0% for cyromazine, and the relative standard deviation was not over 2.0%. The cyromazine concentration ranged from 92.7% to 109.4% and was within the acceptable range (90~120%) for the percent of the labeled amount. This method was found to be suitable for determining cyromazine in commercial insecticides.

• Textile Coloration and Finishing
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• v.32 no.4
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• pp.217-225
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• 2020

In this study, the dyeing characteristics of nylon fabric which is dyed with supercritical fluid were investigated. There were two dyes used in the dyeing experiment: C.I. Disperse Red 167 and C.I. Disperse Violet 93. Dyeing temperature, pressure, and leveling time were fixed at 110℃, 250bar, 60minutes, and the experiment was conducted with dyeing concentration of 0.1, 0.3, 0.5, and 0.85% o.w.f. The analysis of the experimental results was found out through the measurement of washing fastness and color coordinate. In addition, the calibration curve of each dye was drawn up and the amount of remaining dye was checked by measuring the absorbance of the residual dye. As a result of color difference measurement, as the concentration increased, the L⁎ value decreased and the K/S value increased. However, the increase in K/S value compared to the amount of input decreased as the concentration increased. The comparative experiment on the amount of residual dye(C.I. Disperse Red 167) in the pot showed that 99.14% of the amount was dyed at the concentration of 0.1% o.w.f, while it rapidly decreased to 77% at 0.85% o.w.f. C.I. Disperse Violet 93 dye also decreased from 0.5% o.w.f to 93.91%. In the washing fastness experiment of both dyes, the level of washing fastness began to decrease from samples dyed at 0.5% o.w.f. It may be because the simply absorbed dye was produced instead of completely being fixed in the amorphous region of the nylon fiber.

• 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.

• Korean Journal of Ecology and Environment
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• v.40 no.2
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• pp.201-213
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• 2007

In this study, the Batter Assessment Science Integrating point and Nonpoint Sources (BASINS 3.0)/window interface to Hydrological Simulation Program-FPRTRAN (WinHSPF) was applied for assessment of Soyang Dam watershed. WinHSPF calibration was performed using monitoring data from 2000 to 2004 to simulate stream flow. Water quality (water temperature, DO, BOD, nitrate, total organic nitrogen, total nitrogen, total organic phosphorus and total phosphorus) was calibrated. Calibration results for dry-days and wet-days simulation were reasonably matched with observed data in stream flow, temperature, DO, BOD and nutrient simulation. Some deviation in the model results were caused by the lack of measured watershed data, hydraulic structure data and meteorological data. It was found that most of pollutant loading was contributed by nonpoint source pollution showing about $98.6%{\sim}99.0%$. The WinHSPF BMPRAC was applied to evaluate the water quality improvement. These scenarios included constructed wetland for controlling nonpoint source poilution and wet detention pond. The results illustrated that reasonably reduced pollutant loadin. Overall, BASINS/WinHSPF was found to be applicable and can be a powerful tool in pollutant loading and BMP efficiency estimation from the watershed.

• Applied Biological Chemistry
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• v.48 no.3
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• pp.267-272
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• 2005

trans-Cinnamaldehyde, a major component of Cinnamomum cassia, was quantitatively analyzed using the $^1H-NMR$ spectrometry. Applicability of this method was confirmed through observing the variation of chemical shift in the $^1H-NMR$ spectrum of t-cinnamaldehyde and the integration value according to various sample concentrations or running temperatures. When the $^1H-NMR$ spectrometry was run for t-cinnamaldehyde (7.1429 mg/ml) at 19, 25, 30, 40 and $50^{\circ}C$, the chemical shifts of the doublet methine signal due to an aldehyde group were observed at 9.7202, 9.7184, 9.7169, 9.7142 and 9.7124 ppm, respectively, to imply that the running temperature had no significant variation in the chemical shift of the signal. The integration values of the signal were $1.37\;(19^{\circ}C),\;1.37\;(25^{\circ}C),\;1.37\;(30^{\circ}C),\;1.37(40^{\circ}C)$ and $1.37(50^{\circ}C)$, respectively, to also indicate running temperature gave no effect on the integration value. When the sample solutions with various concentrations such as 0.4464, 0.8929, 1.7857, 3.5714, 7.1429 and 14.286 mg/ml were respectively measured for the $^1H-NMR$ at $25^{\circ}C$, the chemical shifts of the aldehyde group were observed at 9.7206, 9.7201, 9.7196, 9.7192, 9.7185 and 9.7174 ppm. Even though the signal was slightly shifted to the high field in proportion to the increase of sample concentration, the alteration was not significant enough to applicate this method. The calibration curve for integration values of the doublet methine signal due to the aldehyde group vs the sample concentration was linear and showed very high regression rate ($r^2=1.0000$). Meantime, the $^1H-NMR$ spectra (7.1429 mg/ml $CDCl_3,\;25^{\circ}C$) of t-cinnamaldehyde and t-2-methoxycinnamaldehyde, another constituent of Cinnamomum cassia, showed the chemical shifts of the aldehyde group as ${\delta}_H$ 9.7174 (9.7078, 9.7270) for the former compound and ${\delta}_H$ 9.6936 (9.6839, 9.7032) for the latter one. The difference of the chemical shift between two compounds was big enough to be distinguished using the NMR spectrometer with 0.45 Hz of resolution. The contents of cinnamaldehyde in Cinnamomum cassia, which were respectively extracted with n-hexane, $CHCl_3$, and EtOAc, were determiend as 94.2 \;mg/g (0.94%), 137.6 mg/g (1.38%) and 140.1 mg/g(1.40%) t-cinnamaldehyde in each extract, respectively, by using the above method.

• Bulletin of the Korean Chemical Society
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• v.33 no.2
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• pp.553-558
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• 2012

A simple new method was developed for the determination of betaine in Fructus Lycii using hydrophilic interaction liquid chromatography with evaporative light scattering detection (HILIC-ELSD). Good chromatographic separation and reasonable betaine retention was achieved on a Kinetex HILIC column ($2.1{\times}100mm$, $2.6{\mu}m$) packed with fused-core particle. The mobile phase consisted of (A) acetonitrile and (B) 10 mM ammonium formate (pH 3.0)/acetonitrile (90/10, v/v). It was used with gradient elution at a flow rate of 0.7 mL/min. The column temperature was set at $27.5^{\circ}C$ and the injection volume was $10{\mu}L$. The ELSD drift tube temperature was $50^{\circ}C$ and the nebulizing gas (nitrogen) pressure was 3.0 bar. Stachydrine, a zwitterionic compound, was used as an internal standard. Calibration curve over $10-250{\mu}g/mL$ showed good linearity ($R^2$ > 0.9992) and betaine in the 70% methanol extract of Fructus Lycii was well separated from other peaks. Intraand inter-day precision ranged from 1.1 to 3.0% and from 2.4 to 5.3%, respectively, while intra- and inter-day accuracy ranged from 100.0 to 107.0% and from 94.3 to 103.9%, respectively. The limit of quantification (LOQ) was $10{\mu}g/mL$ and the recoveries were in the range of 98.2-102.7%. The developed HILIC-ELSD method was successfully applied to quantitatively determine the amount of betaine in fourteen Fructus Lycii samples from different locations, demonstrating that this method is simple, rapid, and suitable for the quality control of Fructus Lycii.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.50 no.spc1
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• pp.211-215
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• 2005

Three curcuminoids [curcumin (CUR), demethoxycurcumin(DEM), bisdemethoxycurcu in (BIS)] are major yellow pigments in turmleric (Curcuma longa L.) root. Contents of curcuminoids in turmeric roots collected from 6 locations were analyzed using, high performance liquid chromatography (HPLC) equipped with reversed-phase column, an UV-Vis detector at 420nm, and eluted with a mixture of acetonitrile: $0.1\%$ acetic acid in water (50 : 50, v/v) as mobile phase. The stability of curcuminoid pigments in $80\%$ methanol extract solution were investigated during storage in a freezer at $-20^{\circ}C$, room temperature in the dark, and light condition. Calibration curves for the determination of curcuminoids were made with significant linearity $(r^2=0.999**)$. Average content of total curcuminoids was 171.5 mg/g, with 91.6 mg/g of CUR, 56.9 mg/g of DEM, and 23.0 mg/g of BIS. Amount of curcuminoids during storage in a freezer was almost not changed while those in room temperature wert reduced and rapid degradation appeared after 60 days. Within 90 days, about $50\%$ curcuminoid decreased in the dark and about $70\%$ in the light condition, indicating the decomposition of curcuminoid pigments followed under light and heat.

• Korean Journal of Ecology and Environment
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• v.37 no.2 s.107
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• pp.205-212
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• 2004

Phosphorus cycle was studied in a deep stratified reservoir in summer monsoon area (Lake Soyang, Korea) by surveying phosphorus input from the watershed and the movement of phosphorus within the reservoir. And the spatial and temporal distribution of phosphorus was modeled with a 2-dimensional water quality model (CE-QUAL-W2), Phosphorus loading was calculated by measuring TP in the main inflowing river (the Soyang River) accounting for 90% of watershed discharge. TP of the Soyang River showed a large daily variation with the flow rate. High phosphorus loading occurred during a few episodic storm runoff laden with suspended sediments and phosphorus. Because storm runoff water on rainy days have lower temperature, it plunges into a depth of same temperature (usually below 20m depth), forming an intermediate turbidity layer with a thickness of 20 ${\sim}$ 30 m. Because of stable thermal stratification in summer the intermediate layer water of high phosphorus content was discharged from the dam through a mid-depth outlet without diffusing into epilimnion. The movement of runoff water within the reservoir, and the subsequent distribution of phosphorus were well simulated by the water quality model showing a good accuracy. The major parameter for the calibration of phosphorus cycle was a settling velocity of detritus, which was calibrated to be 0.75 m ${\cdot}$ $day^{-1}$. It is concluded that the model can be a good simulator of limnological phenomena in reservoirs of summer monsoon area.

• Journal of Korea Water Resources Association
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• v.50 no.12
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• pp.837-847
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• 2017

Land Surface Model (LSM) was developed for the Soyang river basin located in Korean Peninsula to clarify the spatio-temporal variability of hydrological weather parameters. Variable Infiltration Capacity (VIC) model was used as a LSM. The spatial resolution of the model was 10 km and the time resolution was 1 day. Based on the daily flow data from 2007 to 2010, the 7 parameters of the model were calibrated using the Isolated Particle Swarm Optimization algorithm and the model was verified using the daily flow data from 2011 to 2014. The model showed a Nash-Sutcliffe Coefficient of 0.90 and a correlation coefficient of 0.95 for both calibration and validation periods. The hydrometeorological variables estimated for the Soyang river basin reflected well the seasonal characteristics of summer rainfall concentration, the change of short and shortwave radiation due to temperature change, the change of surface temperature, the evaporation and vegetation increase in the cover layer, and the corresponding change in total evapotranspiration. The model soil moisture data was compared with in-situ soil moisture data. The slope of the trend line relating the two data was 1.087 and correlation coefficient was 0.723 for the Spring, Summer and Fall season. The result of this study suggests that the LSM can be used as a powerful tool in developing precise and efficient water resources plans by providing accurate understanding on the spatio-temporal variation of hydrometeorological variables.