• Archives of Pharmacal Research
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• v.26 no.2
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• pp.120-123
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• 2003

A method for the determination of terbutaline enantiomers in human urine by capillary elctrophoresis has been developed. Optimum resolution was achieved using 50 mM phosphate buffer, pH 2.5, containing 15 mM of hydroxypropyl-$\beta$-cyclodextrin as a chiral selector. Urine samples were prepared by solid-phase extraction with Sep-pak silica, followed by CE. The assay was linear between 2-250 ng/mL (R = 0.9998 for (S)-(+)-terbutaline and R = 0.9999 for (R)-(-)-terbutaline) and detection limit was 0.8 ng/mL. The intra-day variation ranged between 6.3 and 14.5% in relation to the measured concentration and the inter-day variation was 8.2-20.1%. It has been applied to the determination of (S)-(+)-terbutaline and (R)-(-)-terbutaline in urine from healthy volunteer dosed with racemic terbutaline sulfate.

• Bulletin of the Korean Chemical Society
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• v.29 no.7
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• pp.1323-1325
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• 2008

The acetylene black (AB) was dispersed into water in the presence of dihexadecyl hydrogen phosphate (DHP) via ultrasonication, resulting in a stable and well-distributed AB/DHP suspension. After evaporation of water, an AB/DHP composite film-modified electrode was prepared. The electrochemical responses of $K_3$[Fe$(CN)_6$] at the unmodified electrode, DHP film-modified electrode and AB/DHP film-modified electrode were investigated. It is found that the AB/DHP film-modified electrode possesses larger surface area and electron transfer rate constant. Furthermore, the electrochemical behaviors of 1-naphthylacetic acid (NAA) were examined. At the AB/DHP film-modified electrode, the oxidation peak current of NAA remarkably increases. Based on this, a sensitive and convenient electrochemical method was proposed for the determination of NAA. The linear range is in the range from $4.0 {\times} 10^{-8}\;to\;5.0 {\times} 10^{-6}$ mol $L^{-1}$, and the detection limit is $1.0 {\times} 10^{-8}$ mol $L^{-1}$. Finally, this new sensing method was employed to determine NAA in several soil samples.

• YAKHAK HOEJI
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• v.44 no.2
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• pp.135-140
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• 2000

Determination of Aconitum alkaloids in processed Buza (Cho-0, Salted Buza, Moist-heating Buza, Limed Buza), which had been prepared from the raw tubers of Aconitum chiisanenseb(Ranunculaceae), was established using visible spectrophotometry and high-performance liquid chromatography (HPLC) method especially for Aconitine analysis. Aconitum alkloids were reacted with tetra- thiocy-anatocobalt[II] complex ion to form a stable ion pair. The reaction product was insoluble in water but freely soluble in several organic solvents. 1.2-Dichloroethane was the best extracting solvent among the examined solvents. Spectrophotometry of Aconitum alkaloids at nax. 625 was carried out. The HPLC method for aconitine was carried out using Radial PAK-CN column with gradient solvent system by solvent mixture of acetonitrile and phosphate buffer (pH 3.0) at 4$0^{\circ}C$ and 254 nm. Linear relationship was found between absorbance response and concentration of aconitine in range of 0.45 mM~0.9 mM ($r^2$=0.9949) by spectrophotometry and 0.3 mM~1.2mM($r^2$=0.9983) by HPLC method. These methods have been found to be suitable and reproducible for routine analysis of Aconitum alkaloids and its pharmaceutical preparations.

• Journal of Veterinary Clinics
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• v.8 no.1
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• pp.31-45
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• 1991

Present experiment was performed in order to establish the optimal reaction conditions for determination of urinary AAP and GRS activities and to investigate the applicability of urinary AAP and GRS in nephrotoxicity test in rat. The results were as follows ; 1. The optimal pH of phosphate buffer for determination of urinary AAP activity was 7.8. 2. The Michaelis constant of urinary AAP ranged from 0.8 to 1.0mmol/$\ell$ 3. The optimal wave length for determination of urinary GRS activity was 405nm. 4. The optimal pH of acetate buffer for determination of urinary GRS activity was 5.6. 5. The Michaelis constant of urinary GRS ranged from 0.65~0.79mmo1/$\ell$. 6. The AAP activities in gel-filtered samples were significantly higher than those in crude samples. Mean values of AAP activities in gel-filtered samples and crude samples were 29$\pm$20 and 20$\pm$13U/$\ell$, respectively. 7. There was not significant difference between gel-filtered samples and crude samples in urinary GRS activities. Mean values of GRS activities in gel-filtered samples and crude samples were 57$\pm$40 and 56$\pm$39U/$\ell$, respectively. 8. Limits of linearity of urinary AAP and GRS activities were 2.0 and 3.6U/$\ell$, respectively. 9. Within-run imprecisions of the assays, were acceptable, as the coefficients of the AAP activities ranged from 5.5 to 6.3% and those of GRS activities ranged from 1.4 to 6.2%, respectively. 10. Urinary AAP excretion was 675$\pm$227mu/24hrs.kg before administration of potassium dichromate, and increased significantly to 4246$\pm$2567mU/24hrs.kg within 24 hours after administration of potassium dichromate. 11. Urinary GRS excretion did not increase significantly after administration of potassim dichromate. 12. From these findings it is concluded that urinary AAP excretion is early and sensitive Indicator to detect kidney damage in nephrotoxicity experiment.

• Analytical Science and Technology
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• v.14 no.2
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• pp.103-108
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• 2001

Rare earth elements(REE) were separated by solvent extraction with tri-n-butyl phosphate(TBP) and $NaNO_3$, followed by back extraction with water. The method was applied to the determination of REE to circumvent the spectral interferences of ICP-AES analysis. The effects of the $NaNO_3$ concentration and the addition of hydrophobic solvents on the extraction efficiencies were investigated. Increases of the $NaNO_3$ concentration enhanced the extraction efficiencies of REE, and more than 95% recoveries were obtained at 5M of $NaNO_3$ concentration. On the other hand, addition of hydrophobic solvents lowered the extraction efficiencies. The method was applied to determine the REE in the monazite sample. But the precisions of the analytical results were more than 20%.

• Bulletin of the Korean Chemical Society
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• v.26 no.9
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• pp.1403-1409
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• 2005

A sensitive and selective electrochemical method was developed for the amperometric determination of ascorbic acid (AA) at a glassy carbon electrode (GCE) modified with single-wall carbon nanotubesdihexadecyl hydrogen phosphate (SWNT-DHP) composite film. The SWNT-DHP composite film modified GCE was characterized with SEM. The SWNT-DHP composite film modified GCE exhibited excellent electrocatalytic behaviors toward the oxidation of AA. Compared with the bare GCE, the oxidation current of AA increased greatly and the oxidation peak potential of AA shifted negatively to about -0.018 V (vs. SCE) at the SWNT-DHP composite film modified GCE. The experimental parameters, which influence the oxidation current of AA, were optimized. Under the optimal conditions, the amperometric measurements were performed at a applied potential of -0.015 V and a linear response of AA was obtained in the range from 4 ${\times}$ $10^{-7}$ to 1 ${\times}$ $10^{-4}$ mol $L^{-1}$ and with a limit of detect (LOD) of 1.5 ${\times}$ $10^{-7}$ mol $L^{-1}$. The interferences study showed that the SWNT-DHP composite film modified GCE exhibited good sensitivity and excellent selectivity in the presence of high concentration uric acid and dopamine. The proposed procedure was successfully applied to detect AA in human urine samples with satisfactory results.

• Journal of the Korean Chemical Society
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• v.32 no.5
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• pp.422-427
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• 1988

The bio-electrode for L-asparagine, excellent in the reproducibility of responsibility, has been constructed by immobilizing the bacterium Proteus mirabilis on an ammonia gas sensor. This electrode was investigated for the effects of pH, temperature, buffer solution, bacterial amounts and interferences, and stability with the lapse of time. The response of the bacterial electrode was linear in the range of $9.0{\times}10^{-5}$ ∼ $1.0{\times}10^{-2}M$ L-asparagine with a slope of 58.9mV/decade in pH 7.8, 0.05M phosphate buffer solution at $30^{\circ}C$. The bacterial amounts used for this electrode was 3 mg and response time was 7∼9 min. Therefore, this assembly can be used for the determination of L-asparagine.

• Journal of the Korean Chemical Society
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• v.33 no.3
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• pp.304-308
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• 1989

The spectrophotometric determination of $Lu^{3+},\;Eu^{3+}$ and some other rare earths have been investigated using Methyl Thymol Blue(MTB) as spectrophotometric reagent. Rare earth elements form a stable complex with MTB abount pH 6.5 and the ratio of its complex is 1 to 1. MTB has a absorption maxima at 440nm and rare earth MTB complex has absorption maxima 610nm at pH 6.5, respectively. The absorbance of the rare earth MTB complex is stable in 7 hours after color developing and obey the Beer law in the range of $0{\sim}110{\mu}g/50ml$. The ligand such as phosphate, citrate and EDTA decrease the absorbance of its complex considerably, and this method has a poor selectivity of each rare earth element and the molar absorptivity is $1.2{\sim}2.0{\times}10^4mol^{-1}{\cdot}l{\cdot}cm^{-1}$. In methyl alcohol, ethyl alcohol and acetone medium we did not find out any absorption change of the rare earth MTB complex.

• Archives of Pharmacal Research
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• v.23 no.2
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• pp.178-181
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• 2000

In order to study the simultaneous determination of (+)- and (-)-cetirizine in human urine we have developed a chiral separation method by HPLC. A chiral stationary phase of $\alpha$$_1$-acidglycoprotein, the AGP-CSP was used to separate the enantiomers. The pH of the phosphate buffer, as well as the content of the organic modifier in the mobile phase, markedly affected the chromatographic separation of (+)- and (-)-cetirizine. A mobile phase of 10 m㏖/1 phosphate buffer (pH 7.0)-acetonitrile (95 : 5, v/v) was used for the urine assays. Ultraviolet absorption was monitored at 230nm and roxatidine was employed as the internal standard for quantification. (+)-Cetirizine, (-)-cetirizine and the internal standard were eluted at retention times of 12, 16, and 32 mins, respectively. The detection limit for cetirizine enantiomers was 400 ng/$m\ell$ of urine. A pharmacokinetic study was conducted with the help of 5 healthy female volunteers who were administered with a single oral dose of racemic cetirizine (20 mg). The peak area ratios provided by the cetirizine enantiomers were linear(r>0.997) over a concentration range of 2.5-200 ${\mu}g/ml$. The peak of the excreted cetirizine enantiomers appeared in the urine sample during the period of 1-2 hrs following the administration of the oral dose. The excreted level of (+)-cetirizine was slightly higher than (-)-cetirizine but the difference was not statistically significant. However, this method appears to have applications for enantioselective pharmacokinetic studies of racemic drugs.

• Korean Journal of Soil Science and Fertilizer
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• v.42 no.3
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• pp.192-200
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• 2009

Soil testing is one of the best management practices for sustainable agriculture. Recently, as increasing soil testing needs, simplification of soil analytical procedure has been required. To determine recommendable multi-element extractant, the soil testing results of available phosphate and exchangeable cations between the conventional methods (Lancaster and 1M $NH_4OAc) and multi-element extraction methods such as Mehlich III, Modified Morgan and Kelowna methods were compared. There were highly significant correlation between the conventional methods and multi-element extraction methods (Mehlich III, Modified Morgan and Kelowna) for available phosphate and exchangeable K, Ca, Mg and Na. The coefficients of determination ($R^2) between available phosphate extracted by Lancaster method and multielement extraction methods were in the order of Mehlich III ($0.979^{***}$) > Kelowna ($0.977^{***}$) > Modified(Mod.). Morgan ($0.553^{***}$). For exchangeable cations, there were highly significant correlations between 1M $NH_4OAc method and Mehlich III, Mod. Morgan and Kelowna. However, exchangeable K, Ca and Mg by Mehlich III method were more highly correlated with conventional method than other methods. Therefore, Mehlich III extraction method could be recommended as a single extractant for simultaneous measurement using ICP in the analysis of avaliable phosphate and exchangeable cations.