• Analytical Science and Technology
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• v.37 no.4
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• pp.211-219
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• 2024

This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R² > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

• Mass Spectrometry Letters
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• v.11 no.1
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• pp.10-14
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• 2020

Riboflavin is a water-soluble vitamin, which serves as a precursor to flavin mononucleotide and flavin adenine dinucleotide. This study aimed to develop a simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis for the quantification of riboflavin in the Beagle dog plasma. This method utilized simple protein precipitation with acetonitrile and ¹³C₄, ¹⁵N₂-riboflavin was used as an internal standard (IS). For chromatographic separation, a hydrophilic interaction liquid chromatography (HILIC) column was used with gradient elution. The mobile phase consisted of 0.1% (v/v) aqueous formic acid with 10 mM ammonium formate and acetonitrile with 0.1% (v/v) formic acid. Since riboflavin is an endogenous compound, 4% bovine serum albumin in phosphate buffered saline was used as a surrogate matrix to prepare the calibration curve. The quantification limit for riboflavin in the Beagle dog plasma was 5 ng/mL. The method was fully validated for its specificity, sensitivity, accuracy and precision, recovery, and stability according to the US FDA guidance. The developed LC-MS/MS method may be useful for the in vivo pharmacokinetic studies of riboflavin.

• Analytical Science and Technology
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• v.29 no.5
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• pp.234-241
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• 2016

The approach presented in this article refers to the bioanalytical method validation for the detection and quantitative determination of arsenic species including arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) in dog plasma by high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS). The arsenic species were separated using an agilent As speciation column by a mobile phase of 2 mM sodium phosphate monobasic, 0.2 mM ethylenediaminetetraacetic acid disodium salt dehydrate, 10 mM sodium acetate, 3 mM sodium nitrate and 1 % ethyl alcohol at pH 11 (adjusted with 1M NaOH). The method validation experiment was obtained selectivity, linearity, accuracy, precision, matrix effect, recovery, system suitability, dilution integrity and various stabilities. All calibration curves showed good linearity (R²>0.999) within test ranges. The lower limit of quantitation (LLOQ) was 5 ng/mL for As(III), As(V) and DMA, and 20 ng/mL for MMA. The system suitability and dilution values were within 6.5 % and 7.7 %. Subsequently, the developed and validated HPLC-ICP/MS method was also successfully applied to determine the arsenic speciation in dog plasma samples, and the recoveries for the spiked samples were in the range of 91.5–102.2 %. Therefore, this method could be applied to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies in biological samples.

• Korean Journal of Veterinary Service
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• v.45 no.3
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• pp.243-248
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• 2022

The HPLC conditions for analysis of ivermectin in solutions dosage forms of commercial anthelmintics are different for each product. The purpose of this study was to establish a standardized chromatographic method for the quantification of ivermectin in solution. The separation was achieved on Waters Xbridge C18 column (4.6×150 nm, 5 ㎛) using different kinds of mobile phase composed of water/methanol/acetonitrile (15/34/51, v/v and 19.5/27.5/53, v/v), with UV detection at wavelengths 245 nm and 254 nm. A total of five commercial ivermectin in solution samples were analyzed. In this study, the optimal chromatographic conditions for analysis of ivermectin in solution were mobile phase of water/methanol/acetonitrile (15/34/51, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 245 nm using a Waters Xbridge C18 column (4.6×250 nm, 5 ㎛) at a column temperature of 25℃. The linearity was observed in the concentration range of 50~150 ㎍/mL, with a correlation coefficient, r²= 0.99999. The limit of detection and the limit of quantification were 0.88 and 2.68 ㎍/mL, respectively. The accuracy (% recovery) was found to be 98.9 to 100.3%. Intra-day and Intermediate precisions with relative standard deviations were less than 1.0%. The content of ivermectin for five market samples ranged 91.2~102.7%. The proposed method was also found to be robust, therefore, the method can be used for the routine analysis of ivermectin in solutions dosage forms.

• Journal of IKEEE
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• v.24 no.3
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• pp.853-858
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• 2020

This paper proposes a 2-ch DC-DC converter for OLED display with immunity against RF noise inserted from communication device. For RF signal immunity, an input voltage variation reduction circuit that attenuates as much as the input voltage variation is embedded. The boost converter for positive voltage V_POS operates in SPWM-PWM dual mode and has a dead time controller to increase power efficiency. The inverting charge pump for negative voltage V_NEG is a 2-phase scheme and operates in PFM using VCO to reduce output ripple voltage. Simulation results using 0.18 ㎛ BCDMOS process show that the overshoot and undershoot of the output voltage decrease from 10 mV to 2 mV and 5 mV, respectively. The 2-ch DC-DC converter has power efficiency of 39%~93%, and the power efficiency of the boost converter is up to 3% higher than the conventional method without dead time controller.

• Analytical Science and Technology
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• v.8 no.1
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• pp.17-23
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• 1995

The determination method of 2-mercapto-1-methyl-imidazole(MMI) in $5.0{\times}10^{-2}M$ lithium perchlorate solution has been investigated by the differential pulse polarography. The optimum conditions for the determination of MMI were as fellows; -0.9 volt(vs. Ag/AgCl) initial potential, 80mV pulse height, 2mV/sec scan rate, and medium mercury drop size. The calibration curve showed a good linearlity in the range of $1.0{\times}10^{-7}M$ to $8.0{\times}10^{-5}M$ and the detection limit was $2.2{\times}10^{-9}M$. This method was applicable to the determination of MMI in thyroid drugs without interference from the additives.

• Advances in nano research
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• v.5 no.4
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• pp.373-392
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• 2017

Silver nanoparticles (AgNPs) were successfully synthesized through a simple green route using the Nelumbo nucifera leaf, stem and flower extracts. These nanoparticles showed characteristic UV-Vis absorption peaks between 410-450 nm which arises due to the plasmon resonance of silver nanoparticles. The Fourier transform infrared spectroscopy (FT-IR) confirmed the presence of amides and which acted as the stabilizing agent. X-ray diffraction spectrum of the nanoparticles confirmed the Face centered cubic (FCC) structure of the formed AgNPs. Dynamic light scattering technique was used to measure hydrodynamic diameter (68.6 nm to 88.1 nm) and zeta potential (-55.4 mV, -57.9 mV and 98.9 mV) of prepared AgNPs. The scanning electron micrographs of dislodged nanoparticles in aqueous solution showed the production of reasonably monodispersed silver nanoparticles (1-100 nm). The antimicrobial activity of prepared AgNPs was evaluated against fungi, Gram-positive and Gram-negative bacteria using disc diffusion method. Anti-corrosion studies were carried out using coupon method (mild steel and iron) and dye degradation studies were carried out by assessing photo-catalytic activity of Nelumbo nucifera extracts mediated AgNPs.

• 한국정보디스플레이학회:학술대회논문집
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• 2007.08a
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• pp.486-489
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• 2007

Carbon nanotube (CNT) cathodes having a trench structure similar to the structure of the gated triodetype cathode were successfully fabricated by a screenprinting method with multi-walled carbon nanotubes. We observed that a liquid method not only readily removes the organic residues on the CNT films, but also satisfactorily protrudes the CNTs out of the electrode surface. The CNT cathodes prepared by the liquid method showed a turned-on field of $1.4\;V/{\mu}m$. The emission current density of them was about $3.1\;mA/cm^2$ at the electric field of $3\; V/{\mu}m$. The liquid method appears to be a promising surface treatment of CNT cathode for gated triode-type FEDs applications.

• Journal of the Korean Ceramic Society
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• v.26 no.2
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• pp.210-220
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• 1989

The properties of the powder of Al2O3-15v/o ZrO2(＋3m/o Y2O3) system prepared by co-precipitation method at the pH values of 7, 9, 10 and 11 were investigated. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Zirconium hydroxide decreased the specific surface area of aluminum hydroxide of AlOOH type, while increased the specific surface area of aluminum hydroxide of Al(OH)3 type, and formed co-network structure of Al-O-Zr type with the aluminum hydroxides. The rate of transition to $\alpha$-Al2O3 from co-precipitated materials occurred in the order of 7≒10, 9 and 11 of pH values. Al2O3 and ZrO2 interacted to bring about coupled grain growth, and the growth of ZrO2 crystallite size rapidly occurred within $\theta$-Al2O3 matrix. Segregation did not occur in the system Al2O3-15v/o ZrO2(＋3m/o Y2O3) and Y2O3 acted as a stabilizer to ZrO2. The lattice strain of tetragonal ZrO2 was increased by the constraint effect of Al2O3 matrix.

• Bulletin of the Korean Chemical Society
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• v.19 no.9
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• pp.927-933
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• 1998

Polycrystalline powder of vanadium-doped forsterite (Vδ $Mg_2SiO_4$) was synthesized by the $H_2O_2$-assisted sol-gel method. The vanadium dopant, which was added as VO$(OMe)_3$ in methanol, went through several redox reactions as the sol-gel reaction proceeded. Upon adding VO$(OMe)_3$ to a mixture of $Mg(OMe)_2$ and Si$(OEt)_4$ in methanol, V(V) reduced to V(IV). As hydrolysis reaction proceeded, the V(IV) oxidized all back to V(V). Apparently, some of the V(V) reduced to V(IV) during subsequent gelation by condensation reaction. The V(IV) remained even after heat treatment of the gel in highly oxidizing atmosphere. The crystallization of the xerogel around 880 ℃ readily produced single phase forsterite without any minor phase. Using the polycrystalline powder as feeding stock, single crystals of vanadium-doped forsterite were grown by the floating zone method in oxidizing or reducing atmosphere. The doping was limited in low level because of the high partitioning of the vanadium in liquid phase during melting. The greenish single crystal absorbed visible light of 700∼1100 nm. But, no emission was obtained in near infrared range.