• Analytical Science and Technology
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• v.8 no.2
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• pp.215-220
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• 1995

A simple, efficient and sensitive method was described for the simultaneous determination of catecholamine, indoleamine and related metabolites from the homogenates of the rat brain striatum by HPLC-ECD. The optimum mobile phase on a reverse phase $C_{18}$ column was 35mM sodium acetate buffer(included 10mM citric acid, 0.13mM $Na_4EDTA$, 0.58mM SOS, pH3-4):MeOH=85:15. The column temperature was $30^{\circ}C$. Dopamine(DA), 3, 4-dihydroxyphenyl acetic acid(DOPAC), homovanilic acid(HVA), 5-hydroxyindole acetic acid(5-HIAA), serotonin(5-HT) and noradrenaline(NA) could be separated and analysed to very small amount. The detection limits of this method were 2~10pg per injection for all components. The effects of age and sex of rat on the contents of the catecholamines and their metabolites in rat brain striatum were studied. The levels of DA and 5-HT contents of the 7 week old female rats were higher than those of the 7 week old male rats. As the age of rat increases, the contents of DOPAC increased significantly.

• Journal of Food Hygiene and Safety
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• v.37 no.5
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• pp.297-305
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• 2022

Antioxidants are food additives that extend the shelf life of food products by preventing lipid rancidity caused by active oxygen. They can either be naturally-derived or manufactured synthetically via chemical synthesis. In this study, method validation of five synthetic antioxidants, namely butylated hydroxyanisole, butylated hydroxytoluene, tertiary butylhydroquinone, propyl gallate, and disodium ethylenediaminetetraacetic acid, was performed using a high performance liquid chromatography-ultraviolet visible detector, and the method applicability was evaluated by analyzing foods containing antioxidants. The coefficient of determination (R²) average was 0.9997, while the limit of detection and limit of quantification were 0.02-0.53 and 0.07-1.61 mg/kg, respectively. The intra and inter-day accuracies and precisions were 83.2±0.7%-98.7±2.1% and 0.1%-5.7% RSD, respectively. Inter-laboratory validation for accuracy and precision was conducted using the Food Analysis Performance Assessment Scheme quality control material. The results satisfied the guidelines presented by the AOAC International. In addition, the expanded uncertainty was less than 16%, as recommended by CODEX. Consequently, to enhance public health safety, the results of this study can be used as basis data for evaluating the intake of synthetic antioxidants and assessing their risks in Korea.

• Environmental Engineering Research
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• v.22 no.2
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• pp.186-192
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• 2017

The carbon paste electrode (CPE) was modified with the pristine bentonite and hybrid material (HDTMA-modified bentonite). The modified-CPEs are then employed as working electrode in an electrochemical detection of As(V) from aqueous solutions using the cyclic voltammetric measurements. Cyclic voltammograms revealed that As(V) showed reversible behavior onto the working electrode. The hybrid material-modified carbon paste electrode showed significantly enhanced electrochemical signal which was then utilized in the low level detection of As(V). Moreover, the studies were conducted at neutral pH conditions. The electrochemical studies were conducted with scan rates (20 to 200 mV/s) to deduce the mechanism of redox processes involved at the electrode surface. The anodic current was linearly increased, increasing the concentration of As(V) from 5.0 to $35.0{\mu}g/g$ using the hybrid material-modified electrode. This provided fairly a good calibration line for As(V) detection. The presence of varied concentrations of As(III) in the determination of total arsenic was studied. The influence of several cations and anions viz., Cu(II), Mn(II), Zn(II), Pb(II), Cd(II), Fe(III), $Cl^-$, $NO_3{^-}$, $PO_4{^{3-}}$, EDTA and glycine in the detection of As(V) from aqueous solution was also studied. Further, in an attempt to simulate the real matrix analysis, the tap water sample was spiked with As(V) and subjected for As(V) detection using the modified-CPE.

• Analytical Science and Technology
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• v.10 no.3
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• pp.187-195
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• 1997

Chemically modified electrodes(CMEs) for Ag(I) were constructed by incoporating 1,5,9,13-tetrathiacyclohexadecane([16]-ane-$S_4$) with a conventional carbon-paste mixture composed of graphite powder and nujol oil. Ag(I) ion was chemically deposited onto the surface of the modified electrode with [16]-ane-$S_4$ by immersion of the electrode in the acetate buffer solution(pH=4.5) containing $5.0{\times}10^{-4}M$ Ag(I) ion. And then the electrode deposited with Ag(I) was reduced at -0.3V vs. S.C.E. Well-defined stripping voltammetric peaks could be obtained by scanning the potential to the positive direction. The CME surface was regenerated with exposure to 0.1M $HNO_3$ solution and was reused for the determination of Ag(I) ion. When deposition/measurement/regeneration cycles were 10 times, the response could be reproduced with relative standard deviation of 6.08%. In case of differential pulse stripping voltammetry, the calibration curve for Ag(I) was linear over the range of $5.0{\times}10^{-7}{\sim}1.5{\times}10^{-6}M$. And the detection limit was $2.0{\times}10^{-7}M$. Various ions such as Cd(II), Ni(II), Pb(II), Zn(II), Mn(II), Mg(II), EDTA, and oxalate(II) did not influence the determination of Ag(I) ion, except Cu(II) ion.

• Bulletin of the Korean Chemical Society
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• v.25 no.2
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• pp.177-181
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• 2004

A PVC membrane electrode for silver ion based on a new cone shaped calix[4]arene (CASCA) as membrane carrier was prepared. The electrode exhibits a Nernstian response for $Ag^+$ over a wide concentration range ($1.0{\times}10^{-1}-8.0{\times}10^{-6}$M) with a slope of 58.2 {\pm}$ 0.5 mV per decade. The limit of detection of the sensor is $5.0{\times}10^{-6}$M. The sensor has a very fast response time (~5 s) in the concentration range of ${\leq}=1.0{\times}10^{-3}$ M, and a useful working pH range of 4.0-9.5. The proposed sensor displays excellent discriminating ability toward $Ag^+$ ion with respect to common alkali, alkaline earth, transition and heavy metal ions. It was used as an indicator electrode in potentiometric titration of $Ag^+$ with EDTA and in direct determination of silver ion in wastewater of silver electroplating.

• Bulletin of the Korean Chemical Society
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• v.26 no.1
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• pp.38-42
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• 2005

Bis(2-methylbenzaldehyde)butane-2,3-dihydrazone(TDSB) was used as new N-N Schiff's base which plays the role of an excellent ion carrier in the construction of a La(III) membrane sensor. The best performance was obtained with a membrane containing, 30% poly(vinyl chloride), 60% benzyl acetate, 6% TDSB and 4% sodium tetraphenyl borate. This sensor reveals a very good selectivity towards La(III) ions over a wide variety of cations, including alkali, alkaline earth, transition and heavy metal ions. The proposed electrode exhibits a Nernstian behavior (with slope of 19.8 mV per decade) over a wide concentration range (1.0 ${\times}$ 10$^{-5}$-1.0 ${\times}$ 10$^{-1}$ M). The detection limit of the sensor is 7.0 ${\times}$ 10$^{-6}$ M. It has a very short response time, in the whole concentration range ($\sim$5 s), and can be used for at least twelve weeks in the pH range of 3.0-9.4. The proposed sensor was successfully applied as an indicator electrode for the potentiometric titration of a La(III) solution, with EDTA. It was also successfully applied in the determination of fluoride ions in three mouth wash preparations.

• Journal of the Korean Chemical Society
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• v.17 no.2
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• pp.126-129
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• 1973

An amperometric method has been developed for the titration of silver with 2,5-dimercapto-1,3,4,-thiadiazole in ammonical solution (1N) using rotating platinum electrode as an indicator electrode and the mercury-mercury (II) iodide as reference electrode. Direct titration of milligram amount of silver (0.05-1.0mg) is possible in the presence of a number of foreign ions in ammonical solution containing ethylenediaminetetraacetic acid as masking agent under atmosphere. The interfering elements are gold and platinum. The milligram amount of silver can be determined by the proposed method within an error ${\pm}3{\%}$.

• Bulletin of the Korean Chemical Society
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• v.23 no.10
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• pp.1394-1398
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• 2002

A novel copper(II) membrane electrode based on diphenylisocyanate bis(acetylacetone) ethylenediimine (DIBAE), as a new hexadentates Schiff's base was prepared. The electrode exhibited a Nernstian response for Cu$^{2+}$ ions over a wide concentration range (1.0 ${\times}$ 10$^{-1}$ to 1.0 ${\times}$ l0$^{-6}$ M) with a limit of detection of 6.0 ${\times}$ 10$^{-7}$ M (39 ppb). The sensor shows a fast response time (15s) and the membrane can be used for more than 4 months without observing any major deviation. The electrode revealed very good selectivity with respect to many cations including alkali, alkaline earth, transition and heavy metal ions. The proposed sensor could be used in a pH range of 3.0-7.5. It was applied to the direct potentiometric determination of copper in black tea, and in wastewater of copper electroplating samples. The electrode was also used in potentiometric titration of the copper(II) ion with EDTA.

• Journal of Electrochemical Science and Technology
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• v.10 no.3
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• pp.321-328
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• 2019

A new miniaturized all solid-state contact Fe (III)-selective PVC membrane electrode based on Fe (II) phthalocyanine as a neutral carrier was described. The effects of the membrane composition and foreign ions on the electrode performance was investigated. The best performance was obtained with a membrane containing 32% poly (vinyl chloride), 64% dioctylsebacate, 3% Fe (II) phthalocyanine, and 1% potassium tetrakis (p-chlorophenyl) borate. The electrode showed near Nernstian response of $26.04{\pm}0.95mV/decade$ over the wide linear concentration range $1.0{\times}10^{-6}$ to $1.0{\times}10^{-1}M$, and a very low limit of detection $1.8{\pm}0.5{\times}10^{-7}M$. The potentiometric response of the developed electrode was independent at pH 3.5-5.7. The lifetime of the electrode was approximately 3 months and the response time was very short (< 7 s). It exhibited excellent selectivity towards Fe (III) over various cations. The miniaturized all solid-state contact Fe (III)-selective membrane electrode was successfully applied as an indicator electrode for the potentiometric titration of $1.0{\times}10^{-3}M$ Fe (III) ions with a $1.0{\times}10^{-2}M$ EDTA and the direct determination of Fe (III) ions in real water samples.

• Korean Journal of Veterinary Research
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• v.36 no.3
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• pp.541-550
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• 1996

Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.