• Journal of the Korean Chemical Society
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• v.8 no.3
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• pp.113-120
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• 1964

The critical examination of the spectrophotometric method for determining microgram quantities of phosphate by the n-butyl acetate extraction as molybdophosphoric acid and subsequent development of the molybdenum blue has been made. In this procedure from 2 to 8 ${\mu}g$. of phosphate-phosphorus can be determined under optimum conditions. The final concentration of ammonium molybdate and the final acidity of perchloric acid for the formation of heteropoly acid are suitable to be ranges of 0.5 to 1.1% and 0. 5 to 1. 1 N respectively, and subsequently extracted with 10 ml. of n-butyl acetate. The extract is developed to molybdenum blue with 5.0 ml. of 1. 3% stannous chloride in 1N hydrochloric acid. The color is stable for at least one hour in the use of perchloric acid for the condensation. In order to determination of submicrogram amounts of phosphate, the sensitivity of the molybdenum blue method is hardly sufficient, a sensitive and stable molybdenum(V)-thiocyanate complex method has been investigated. By the procedure less than 1.2 ${\mu}g$. of phosphate-phosphorus can be determined with an accuracy of less than 5% the relative error. The molybdenum(Ⅵ) extracted by the above procedure is reduced to molybdenum(V) in the extract directly with a solution of 4 to 10% of stannous chloride, 0.5 to 1.5 mM of copper, and 0.1 to 0.9 N of perchloric acid as final concentration in 4.3 to 6.3 N of hydrochloric acid or 9.0 to 13.0 N of sulfuric acid by heating for one minute in boiling water, after cooling, the molybdenum(V)-thiocyanate complex color is developed by adding 6.0 M ammonium thiocyanate solution making the final concentration to be in a range of 0.4 to 0.9 M. This procedure the very sensitive, reliable, and stable can be applied to determining submicrogram amounts of phosphate in natural waters with a precision of 1.6 ${\times}\;10^{-2}$ the standard deviation as absorbance.

• Analytical Science and Technology
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• v.31 no.6
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• pp.225-231
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• 2018

Benzoic acid, methyl paraben, and butyl paraben are preservatives that have been used in pharmaceutical, cosmetic, and food products. However, as their toxicities for human have been reported, many nations and organizations including Korea have established a regulation limit for thier usage of these preservatives in food products. The present study developed the isotope dilution liquid chromatography mass spectrometry method for accurate determination of three target preseratives in soysauce. In this study, the isotope dilution liquid chromatography mass spectrometry method was developed for accurate determination of three target preservatives in soy sauce. LC separation was optimized considering the pKa of benzoic acid which is lower than those of methyl and butyl parabens. A C18 column was used with 5 mM ammonium acetate and methanol as mobile phases. Mass spectrometry was operated in negative mode and selected reaction monitoring mode (SRM). Soy sauce sample was cleaned-up with C18 SPE cartridge for removing matrix inferences and color material. Optimized conditions and the method were validated with soy sauce reference materials for the analysis of food preservatives from Health Science Authority in Singapore. The measured values of benzoic acid, methyl and butyl paraben agreed well with reference values within their uncertainties.

• Journal of Korean Society on Water Environment
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• v.32 no.6
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• pp.649-669
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• 2016

This study explored the analytical conditions for 21 veterinary antibiotics which have been popularly sold in South Korea in 2014 but have not yet been targeted in EPA method 1694. Most of the selected antibiotics were separated by a reverse-phase C18 column with a combination of (buffered) water and organic polar solvent, which was commonly methanol and acetonitrile in the gradient elution mode. Volatile additives such as formic acid, ammonium acetate and ammonium formate were usually added to the mobile phases to minimize asymmetrical and tailing of antibiotics' peaks and to increase their ionization in mass spectrometry. The analytical methods of aminoglycoside antibiotics were distinct from those of the other antibiotics in terms of adoption of ion-pair chromatography (IPC) and hydrophilic interaction liquid chromatography (HILIC) capable of retaining and separating extremely polar compounds due to their hydrophilicity. Trifluoroacetic acid or heptafluorobutyric acid was frequently added to the mobile phase as an ion-pair reagent for the IPC. Tandem mass spectrometry was numerously applied to the detection of antibiotics using positive electrospray ionization (ESI) and the selected reaction monitoring (SRM) mode. All reviewed analytical methods had been/were validated by evaluating recovery, limits of detection and quantification, decision limit or detection capability of the methods.

• Journal of the Korean Applied Science and Technology
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• v.32 no.1
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• pp.85-92
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• 2015

The 50 mole% HCl doped polyaniline(PAni) was synthesized by polymerization of aniline in the presence of hydrochloric acid and ammonium persulfate(APS) as dopant and oxidant, respectively. Then, conducting biodegradable cellulose acetate composite films were also prepared with PAni in acetone to find their applicability to antistatic packaging materials. The tensile strength of PCA05 film with 5 wt% of PAni was decreased by 27% from $377.1kg_f/cm^2$ for CA film itself to $275.2kg_f/cm^2$. Elongation was also decreased from 7.65% to 4.35%. Surface registance of $7.0{\times}10^9{\Omega}/sq$ could be achieved for the PCA containing 5 wt% of PAni. Therefore, this PCA05 film can be applied to antistatic package film for electronic board. In addition, decomposition temperature of these PCA films obtained by thermogravimetric analysis(TGA) was decreased with the amount of PAni in PCA films, and the final weight of char was directly proportional to PAni contents. From this thermal result we can calculate the content of PAni in unknown PCA films.

• Analytical Science and Technology
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• v.27 no.6
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• pp.333-338
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• 2014

A simple and sensitive analytical method for fluoride in urine by ion selective electrode (ISE) method was presented. Traditional buffer for fluoride determination using ISE is acetate-based one. Researchers have pointed out some drawbacks of the buffer for fluoride ISE analysis, and some other buffers including citrate-ammonium buffer and MES buffer have been studied for accurate determination of fluoride in urine here. These buffers provided promising results in environmental field, and this author focused on overcoming the interference of co-existing aluminium. The results show that MES-CyDTA buffer gave the best recovery with accuracy of 95-97.5% and precision of 1.9-7.9% for reference sample of 1.8-7.8 mg/L fluoride in urine, with smaller amount of samples and shorter analysis time compared with the traditional method which used acetate buffer. The method was applied to field samples, and which showed urinary of $0.98{\pm}0.38mg/g$ creatinine for workers in electric cable manufacturing factory (n=15) and $0.59{\pm}0.30mg/g$ creatinine for non-exposed workers (n=12).

• Microbiology and Biotechnology Letters
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• v.22 no.5
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• pp.507-514
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• 1994

Acetyl xylan esterase was produced by E. coli HB101 harboring a recombinant plasmid pKMG6 which contained the estI gene of Bacillus stearothermophilus. The maximum production was observed when the E. coli strain was grown at 37$\circC for 12 hours in the medium containing 0.5% acetyl xylan, 1.0% tryptons, 1.0% sodium chloride, and 0.5% yeast extract. The esterase produced was purified to homogeneity using a combination of ammonium sulfate fractionation, DEAE Sepharose CL-6B ion exchange chromatography and Sephacryl S-200 gel filtration. The native enzyme had an apparent molecular mass of 60 kd and was composed of two identical subunits of 29 kd. The N-terminal amino acid sequence of the polypeptide was Ala-X-Leu-Gln- Ile-Gln-Phe-X-X-Gln. The acetyl esterase displayed a pH optimum of 6.5 and a temperature opti- mum of 45$\circC. The heavy metal ions such as Ag$^{++}$, Hg$^{++}$ and Cu$^{++}$ inhibited nearly completely the activity of the esterase, and no specific metal ion was found to be required for the enzyme activity. The enzyme readily cleaved MAS, $\beta$-D-glucose pentaacetate, $\alpha$-naphthyl acetate, $\rho$-nitrophenyl acetate as well as acetyl xylan, but had no activity on $\rho$-nitrophenyl propionate, $\beta$-nitrophenyl butyrate or $\beta$-nitrophenyl valerate. The Km and Vmax values for MAS were 2.87 mM and 11.55 $\mu$mole/min, respectively. Synergistic behavior was demonstrated with a combination of xylanase and esterase from B. stearothermophilus in hydrolyzing acetyl xylan.

• Journal of the Korean Magnetics Society
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• v.16 no.1
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• pp.107-110
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• 2006

Magnetite nanoparticles encapsulated with biodegradable polymer [poly(D,L-lactide-co-glycoiide), PLGA] were prepared by an emulsification-diffusion method. To investigate the effect of type of organic solvents on the mean particle sizes of obtained composite particles, different organic solvents [ethyl acetate (EA), propylene carbonate (PC) and acetone (ACE)] were used with a stabilizer [didodecyl dimethyl ammonium bromide (DMAB)]. The particle size of nanoparticles was observed by the dynamic light scattering method. When EA and PC as partially water-soluble solvents were used, small composite nanoparticles below 80nm were obtained, while large composite nanoparticles above 330nm were prepared for ACE as a fully water-soluble solvent.

• Microbiology and Biotechnology Letters
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• v.16 no.2
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• pp.105-110
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• 1988

The production of single cell protein using the amylolytic fusant obtained from cell fusion between Hansenula anomala and Saccharomyces cerevisiae was studied. The fusant12 strain was selected for single cell protein production from starchy materials among five fusants. Optimum nitrogen source and its concentration for the growth of fusant12 were ammonium sulfate and 0.1%, respectively. Optimum concentration of soluble starch and optimum pH of the basal medium were lord and pH 5.6, respectively. Autolysis of fusant12 was effectively carried out by addition of 5% (v/v) ethyl acetate to the cell suspension and liquidization for 30 min before incubation for 24 hr at 3$0^{\circ}C$. Coculture of fusant12 and non-amylolytic yeast, Torulopsis candida YA-l5, resulted in the increase of the mass as compared to the monoculture of fusant12. The cell mass on tapioca medium was increased about 2.5 times as on soluble starch medium. The content of crude protein and nucleic acid of the dry cell were 39% and 5.8%, respectively.

• Bulletin of the Korean Chemical Society
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• v.25 no.1
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• pp.109-114
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• 2004

A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

• Proceedings of the Korean Institute of Information and Commucation Sciences Conference
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• 2010.05a
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• pp.805-808
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• 2010

In this paper, CdS thin films, which were widey used window layer of the CdS/CdTe and the CdS/$CuInSe_2$ heterojunction solar cell, were grown by chemical bath deposition, and effects of temperature of reaction solution on the structural properties were investigated. Cadmium acetate and thiourea were used as cadmium and sulfur source, respectively. And ammonium acetate was used as the buffer solution. The reaction velocity was increased with increasing temerature of reaction solution. For temperature <= $85^{\circ}C$, as increasing temperature of solution, deposition rate of CdS films was increased by ion-by-ion reaction in the substrate surface, and the crystallinity of the films was improved. However, for temperature <= $55^{\circ}C$, deposition rate was decreased resulting from smaller Cd2+ ion, and the grain size was decreased.