• Korean Journal of Food Science and Technology
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• v.40 no.2
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• pp.152-159
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• 2008

The purpose of this study was to determine the accurate quantification of vitamin A in infant formula by comparing two different standard stock solutions as well as various sample weights using high performance liquid chromatography. The sources of uncertainty in measurement, such as sample weight, final smaple vloume, and the instrumental results, were identified and used as parameters to determine the combined standard uncertainty based on GUM(guide to the expression of uncertainty in measurement) and the Draft EURACHEM/CITAC Guide. The uncertainty components in measuring were identified as standard weight, purity, molecular weight, dilution of the standard solution, calibration curve, recovery, reproducibility, sample weight, and final sample volume. Each uncertainty component was evaluated for type A and type B and included to calculate the combined uncertainty. The analytical results and combined standard uncertainties of vitamin A according to the two different methods of stock solution preparation were 627 ${\pm}$ 33 ${\mu}$g R.E./100 g for 1,000 mg/L of stock solution, and 627 ${\pm}$ 49 ${\mu}$g R.E./100 g for 100 mg/L of stock solution. The analytical results and combined standard uncertainties of vitamin A according to the various sample weighs were 622 ${\pm}$ 48 ${\mu}$g R.E./100 g, 627 ${\pm}$ 33 ${\mu}$g R.E./100 g, and 491 ${\pm}$ 23 ${\mu}$g R.E./100 g for 1 g, 2 g, and 5 g of sampling, respectively. These data indicate that the preparation method of standard stock solution and the smaple amount were main sources of uncertainty in the analysis results for vitamin A. Preparing 1,000 mg/L of stock solution for standard material sampling rather than 100 mg, and sampling not more than 2 g of infant formula, would be effective for reducing differences in the results as well as uncertainty.

• Journal of the Korean Chemical Society
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• v.4 no.1
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• pp.15-17
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• 1957

1. Preparation of Titanium tetrachloride; The following precesses were strictly followed as the preliminary step to obtain pure $TiOCl_2$, titanyl chloride; First, pure Titanium Oxide mixed with carbon is rolled into pills. After drying up perfectly, these pills are heated at 900∼1000${\circ}C$. And then the pills are subjected to the flow of $Cl_2$ gas in a quartz tube heated to 900-1000${\circ}C$. Thus Titanium tetrachloride is obtained. 2. Preparation of $TiOCl_2$ ; Yellowish trobrown solution is made by pouring 80 g of conc. HCl (sp.gr. 1.19) to 45 gr of Titanium tetrachloride (approx. 2 times of theoretical amount). Then this solution is kept settled for 5-days in a desiccator filled with phosphorous pentoxide at room temperature. As the colorless amorphous solid thus obtained is washed with aceton, 36.5 g of the pure salt are obtained. 3. Determination of composition. The analysis of the sample taken from the deposit desiccated gives the following data; (A) Qualitative analysis; a) $Ti(OH)_4$ is precipitated by adding NaOH in water solution of the salt. b) Adding $AgNO_3$ solution, the water solution of the salt gives white precipitate of AgCl. c) When acid and $H_2O_2$ are added, the solution turns its color to redish brown (This proves that $TiO^{++}$ was converted into $TiO^{++}$ by oxidation of $H_2O_2$. (B) Quantitative analysis; a) $Ti(OH)_4$ precipitated by $10{\%}$ NaOH isalitatsubjected consecutively to the filtration and ignition in porcelain crucible at approx. 1000${\circ}C$. , then $TiO_2$ thus formed is weighed and calculated into Ti content. b) Chlorine involved in water solution of the salt is determined by Vorhardt method. Result: The values obtained from previous analysis, devied by their atomic weight gives the following composition: Ti : Cl = 1 : 2 Therefore $TiOCl_2$ should be given as its molecular formula. 4. Summary. When $TiCl_4$ is additated into conc. HCl, $TiO^{++}$ formed exists as a stable form, and forms $TiOCl_2$. However $TiOCl_2$ is unstable to heating. When the temperature is raised to $65{\circ}C$the decomposition of the solution is accelerated, and gives $TiO_2$ aq. $TiOCl_2$ in addition is highly hygroscopic.

• Journal of Applied Biological Chemistry
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• v.54 no.1
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• pp.1-6
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• 2011

${\gamma}$-PGA(poly-${\gamma}$-glutamic acid) is an unusual anionic polypeptide that is made of D- and L-glutamic acid units connected by amide linkages between ${\alpha}$-amino and ${\gamma}$-carboxylic acid groups. ${\gamma}$-PGA has been isolated from many kinds of organisms. Many Bacillus strains produce ${\gamma}$-PGA as a capsular material of an extracellular viscous material. It is safe for eating as a viscosity element of fermented soybean products such as Chungkookjang and Natto. It is biodegradable, edible and nontoxic toward humans and the environment and its molecular weight varies from ten thousand to several hundred thousand depending on the kinds of strains used. Therefore, potential applications of ${\gamma}$-PGA and its derivatives have been of interest in the past few years in a broad range of industrial fields such as food, cosmetics, medicine, water-treatment, etc. In this study, a bacterium, Bacillus subtilis GS-2 isolated from the Korean traditional seasoning food, Chungkookjang could produce a large amount of ${\gamma}$-PGA with high productivity and had a simple nutrient requirement. Based on carbon utilization pattern and partial 16S rRNA sequence analysis, the GS-2 strain was identified as B. subtilis. The determination of purified ${\gamma}$-PGA was confirmed with thin layer chromatography (TLC), high performance liquid chromatography (HPLC), fourier transform infrared (FT-IR) spectra, and $^1H$-nuclear magnetic resonance ($^1H$-NMR) spectroscopy.

• Journal of Life Science
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• v.29 no.2
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• pp.198-201
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• 2019

Recently, it has been reported that Bacillus mojavensis possesses antifungal properties and plant growth-promoting activities, which are similar to the characteristics of siderophore. In this study, the siderophore produced by B. mojavensis was assessed using a solid phase extraction (SPE) cartridge and liquid chromatography quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). After B. mojavensis was incubated in phenol medium for 16 hr and lyophilized, the sample was dissolved in water and loaded to an SPE cartridge to remove interferences. The cartridge was washed with 5% methanol in water and eluted with 2% formic acid in methanol sequentially. The eluted solution was evaporated under a stream of nitrogen gas and reconstituted in methanol. The reconstituted sample was filtered, and $1{\mu}l$ of the sample was assessed using Q-TOF MS/MS. The mass spectrometer was operated using the positive electrospray ionization mode. Based on the mass spectrum and tandem mass spectrum, the siderophore produced by B. mojavensis was bacillibactin, one of the catechol types of siderophore with a molecular weight of 882.2556. This siderophore analysis could provide a justification for the study of B. mojavensis as a functional food and for pharmaceutical applications.

• Elastomers and Composites
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• v.48 no.2
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• pp.148-155
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• 2013

The crosslinking density of polymer can be quantitatively calculated by the Flory-Rehner equation using the swelling experimental data and the lattice constant ${\beta}_1$ of interaction parameter (${\chi}$) in this equation should be chosen have used cautiously. This ${\beta}_1$ is the experimental data by rule of thumb, and researchers have used little different values respectively. Generally, the average molecular weight between crosslink points $M_c$ in the Flory-Rehner equation and the Mooney-Rivlin equation have the same value, and ${\beta}_1$ can be calculated when the $M_c$ in the Flory-Rehner equation is given. Therefore, in this research, firstly we calculated the $M_c$ using the selected ${\beta}_1$ (=0.34) and the swelling experimental data of 1,2,3-triazole polymer from the Flory-Rehner equation, secondly the $M_c$ from the Mooney-Rivlin equation is calculated by the tensile experimental data, and finally two $M_c$ were compared. As a result, two $M_c$ values were almost the same, and it was proved that the ${\beta}_1$ (=0.34) was selected properly.

• Journal of the Korean Chemical Society
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• v.38 no.9
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• pp.640-652
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• 1994

This work is undertaken to determine alcohol homologues so-called fusel oil that may be present in the Korean folk sojues (distilled liquor) made from grains and to describe sample preparation and analytical method by GC-FID-MS. Solid phase extraction method for sample preparation by using porous styrene divinyl benzene polymer (Porapak Q) was compared with steam distillation and solvent extraction method. Retention behaviors of homologous series of alcohols were also studied. Log values of retention time, molecular weight, boiling point, and capacity factor of alcohols showed linear correlations to the carbon number of an alcohol, to the oven temperature, and to the dielectric constant. Components such as methyl alcohol, n-propyl alcohol, isobutyl alcohol, isopentyl alcohol, and phenethyl alcohol have been identified. The more amount of isopentyl alcohol than other alcohols are contained in the Korean folk sojues, while that of n-propyl alcohol are contained in Chinese kaoliangchiew. Degree of similarity or dissimilarity and classification of the individual samples were discussed using multivariate statistical analysis(principal components analysis) based on GC data.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.4
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• pp.359-364
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• 2014

In this study, we developed a HPLC method for the separation and analysis of methylparaben and p-anisic acid, which are commonly used as a synthetic preservative and natural preservative, respectively. Methylparaben and p-anisic acid have same molecular weight (152.15 g/mol), similar structure and same maximum absorption wavelength (250 nm), thus they showed same retention time (RT) value (13.3 min) in HPLC experiment. We observed that two substances are separated on C18 column after methylparaben was derivatized selectively through the acetylation reaction. Instead, RT of the acetylated methylparaben was moved to 23.9 min from 13.3 min. The average retention time was $23.9{\pm}0.1min$ and peak area values was $5042882{\pm}4778$. In addition it showed a high linearity in the calibration curve with a correlation coefficient (R2) of 0.9999658. Detection and quantitation limits were $1.47{\mu}g/mL$ and $4.44{\mu}g/mL$, respectively. In conclusion, the developed method can be useful for separation and analysis of preservatives with similar structure in cosmetic fields.

• Journal of the Korean Society of Food Science and Nutrition
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• v.33 no.5
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• pp.769-777
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• 2004

A Helicobacter pylori urease inhibitor from Rubus coreanus Miquel has been isolated and partially characterized for aiming to Prevent H. pylori growth and decrease harmful accumulation of ammonia in human gastric mucosa. We screened urease inhibitory activities in 519 extracts library prepared by solvent extraction from 173 kinds of edible plants, medicinal herbs, herbs and seaweeds using a colorimetric urease assay system. As results of primary and secondary screening, 70% acetone extract of Rubus coreanus Miquel was selected as potent candidate, showing about 24% inhibitory activity. The acetone extract was sequentially partitioned into RCE/RCWI and RCB/RCW2 layers with ethyl acetate and butanol. The major active component in RCW2, water layer from butanol fractionation was revealed to be peptidic or proteinous substance by inhibitory activity determination after pronase digestion and periodate oxidation. RCW2-IIIc a was isolated by sequential column chromatography on DEAE-Toyopearl 650C, Butrl-Toyopearl 650M and Sephadex LH-20. The isolated urease inhibitor RCW2-IIIc $\alpha$, was highly pure proteinous substance with molecular weight of 13kDa by high-performance gel permeation liquid chromatography. RCW2-IIIc$\alpha$ has about 5 times higher inhibitory activity than 70％ acetone extract, showing high stability against heat treatment and peptic digestion.

• Korean Journal of Environmental Agriculture
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• v.30 no.2
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• pp.169-178
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• 2011

BACKGROUND: This study aimed to estimate the measurement uncertainty associated with determination of cadmium and lead from tomato paste by ICP/MS. The sources of measurement uncertainty (i.e. sample weight, final volume, standard weight, purity, molecular weight, working standard solution, calibration curve, recovery and repeatability) in associated with the analysis of cadmium and lead were evaluated. METHODS AND RESULTS: The guide to the expression of uncertainty was used for the GUM (Guide to the expression of Uncertainty in Measurement) and Draft EURACHEM/CITAC (EURACHEM: A network of organization for analytical chemistry in Europe/Co-Operation on International Traceability in Analytical Chemistry) Guide with mathematical calculation and statistical analysis. The uncertainty components were evaluated by either Type A or Type B methods and the combined standard uncertainty were calculated by statistical analysis using several factors. Expected uncertainty of cadmium and lead was $0.106{\pm}0.015$ mg/kg (k=2.09) and $0.302{\pm}0.029$ mg/kg (k=2.16), on basis of 95% confidence of Certified Reference Material (CRM) which was within certification range of $0.112{\pm}0.007$ mg/kg for cadmium (k=2.03) and $0.316{\pm}0.021$ mg/kg for lead (k=2.01), respectively. CONCLUSION(s): The most influential components in the uncertainty of heavy metals analysis were confirmed as recovery, standard calibration curve and standard solution were identified as the most influential components causing uncertainty of heavy metal analysis. Therefore, more careful consideration is required in these steps to reduce uncertainty of heavy metals analysis in tomato paste.

• Journal of the Korean Society for Marine Environment & Energy
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• v.17 no.1
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• pp.27-35
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• 2014

The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.