• Journal of Food Hygiene and Safety
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• v.25 no.4
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• pp.388-394
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• 2010

Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.

• Journal of the Korean Geotechnical Society
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• v.15 no.2
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• pp.43-71
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• 1999

This research is an experimental work of developing a construction material using municipal wastewater sludge as liner and cover materials for waste disposal landfill. Weathered granite soil and flyash, produced as a by-product in the power plant, were used as the primary additives to improve geotechnical engineering properties of sludge. For secondary additives, bentonite and cement were mixed with sludge to decrease the permeability and to increase the shear strength, respectively. Various laboratory test required to evaluate the design criteria for liner and cover materials, were carried out by changing the mixing ratio of sludge with the additives. Basic soil properties such as specific gravity, grain size distribution, liquid and plastic limits were measured to analyze their effects on permeability, compaction, compressibility and shear strength properties of mixtures. Laboratory compaction tests were conducted to find the maximum dry densities and the optimum moisture contents of mixtures, and their effectiveness of compaction in field was consequently evaluated. Permeability tests of variable heads with compacted samples, and the stress-controlled consolidation tests with measuring permeabilities of samples during consolidation process were performed to obtain permeability, and to find the compressibility as well as consolidational coefficients of mixtures, respectively. To evaluate the long term stability of sludges, creep tests were also conducted in parallel with permeability tests of variable heads. On the other hand, for the compacted sludge decomposed for a month, permeability tests were carried out to investigate the effect of decomposition of organic matters in sludges on its permeability. Direct shear tests were performed to evaluate the shear strength parameters of mixed sludge with weathered granite, flyash and bentonite. For the mixture of sludge with cement, unconfined compression tests were carried out to find their strength with varying mixing ratio and curing time. On the other hand, CBR tests for compacted specimen were also conducted to evaluate the trafficability of mixtures. Various test results with mixtures were assessed to evaluate whether their properties meet the requirements as liner and cover materials in waste disposal landfill.

• Applied Biological Chemistry
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• v.17 no.2
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• pp.125-137
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• 1974

The chemical structure of glycolipid of Selenomonas ruminantium cell wall was to be elucidated. The bacterial cells were treated in hot TCA and the glycolipid fractions were extracted by the solvent $CHCl_3\;:\;CH_3OH$ (1 : 3). The extracted glycolipids fraction was further separated by acetone extraction. The acetone soluble fraction was named as the spot A-compound. The acetone insoluble but ether soluble fraction was named as the spot B-compound. These two compounds were examined for elucidation of their chemical structure. The results were as follows: 1. The IR spectral analysis showed that O-acyl and N-acyl fatty acids were linked to glucosamine moiety in the spot A-compound. However in the spot B-compound in addition to O and N-acyl acids phosphorus was shown to be attached to glucosamine. 2. It was recognized by gas liquid chromatography that spot A compound contained beta-OH $C_{13:0}$ fatty acid in predominance in addition to the fatty acid with beta-OH $C_{9:0}$, whereas the spot B compound was composed of the predominant fatty acid of beta-OH $C_{13:0}$ with small amount of beta-OH $C_{9:0}$. 3. According to the paper chromatographic analysis of hydrazinolysis products of the spot A compound, a compound of a similar Rf value as the chitobiose was recognized, which indicated a structure of two molecules glucosamine condensed. The low Rf value of the hydrazinolysis product of the spot B-compound confirmed the presence of phosphorus attached to glucosamine. 4. The appearance of arabinose resulting from. ninhydrin decomposition of the acid hydrolyzate of the spot A compound indicated that the amino group is attached to $C_2$ of glucosamine. 5. The amount of glucosamine in the N-acetylated spot A compound decreased in half of the original content by the treatment. with $NaBH_4$, indicating that there are two molecules of glucosamines in the spot A compound. The presence of 1, 6-linkage between two molecules of glucosamine was suggested by the Morgan-Elson reaction and confirmed by the periodate decomposition test. 6. By the action of ${\beta}-N-acetyl$ glucosaminidase the N-acetylated spot A compound was completely decomposed into N-acetyl glucosamine, whereas the spot B compound was not. This indicated the spot A compound has a beta-linkage. 7. When phosphodiesterase or phosphomonoesterase acted on $^{32}P-labeled$ spot B compound, $^{32}P$ was not released by phosphodiesterase, but completely released by phosphomonoesterase. This indicated that one phosphorus is linked to glucosamine moiety. 8. The spot A compound is assumed to have the following chemical structure: That is glucosaminyl, ${\beta}-1$, 6-glucosamine to which O-acyl and N-acyl fatty acids are linked, of which the predominant fatty acid is beta-OH $C_{13:0}$ fatty acid in addition to beta-OH $C_{9:0}$ fatty acid 9. The spot B compound is likely to have the linkage of $glucosaminyl-{\beta}-1$, 6-glucosamine to which phosphorus is linked in monoester linkage. Furthermore both O-acyl and N-acyl fatty acids contained beta-OH $C_{13:0}$ fatty acid predominantly in addition to beta-OH $C_{9:0}$ fatty acid.

• Korean journal of food and cookery science
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• v.12 no.4
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• pp.527-534
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• 1996

enistein (G), and daidzein (D), the major isoflavones, were analyzed in 14 varieties of Korean soybean and various processed soybean products by using high performance liquid chromatography. Isoflavone contents (G+D) were greatly variable among varieties ranged from 308.2 $\mu\textrm{g}$/g to 1,134.2 $\mu\textrm{g}$/g and highest in Danyopkong and Jinpumkong. Among hypocotyl, cotyledon and hull of soybean the concentration of the isoflavone (G+D) in the hypocotyl was highest ranged from 2,971.7 $\mu\textrm{g}$/g to 5,704.9 $\mu\textrm{g}$/g. The distributions of genistein and daidzein were also different in hypocotyl, cotyledon and hull. Higher ratio of daidzein to genistein (D/G) was found in the hypocotyl (4-12) compared to cotyledon and hull (0.1-4). Isoflavone (G+D) contents of soymilks (Sinpaldal#2, Eunhakong) prepared at 16 hour hydration were decreased to 1.1-1.2 times compared with that at 8 hour hydration. Commercial soymilks contained much lower isoflavone (G+D) than laboratory soymilks. Soybean curd (Eunhakong) prepared with MgCl$_2$ showed higher isoflavone (G+D) contents than that with CaSO$_4$. But these values of two different soybean curds made at laboratory were similar to those of 3 commercial curds. The concentration of the isoflavones in soybean sprout separated with 3 parts revealed highest in the head and lowest in the stem. Compared with non-fermented soybean foods the fermented soybean produfts, Kochujang and soybean paste, Duen Jang, showed very low contents of isoflavone (G+D),2.8-3.0 $\mu\textrm{g}$/ｇ, 35.9-63.6 $\mu\textrm{g}$/ｇrespectively.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.327-334
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• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.2
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• pp.203-214
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• 2014

We measured the contact dermatitis-causing substances concentrations in 28 commercial oxidative hair-coloring products. This study was aimed to provide the fundamental data about oxidative hair-coloring products. We selected 10 oxidation dyes (p-phenylenediamine, toluene-2,5-diamine, m-phenylenediamine, nitro-p-phenylenediamine, p-aminophenol, m-aminophenol, o-aminophenol, p-methylaminophenol, N,N'-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 2-methyl-5-hydroxyethylaminophenol) and 4 heavy metal (nikel; Ni, chromium; Cr, cobalt; Co, copper; Cu) as contact dermatitis-causing substances. To identify 10 oxidation dyes, hexane-2% sodium sulfite was used for the rapid and simple extraction and ultra performance liquid chromatography (UPLC) analysis was used for simultaneous analysis in 12 minutes. 10 oxidative dyes were detected as indicated on the product packaging and each concentration was lower than prescribed upper concentration limit by pharmaceutical manufacturing standards. And we analysed inductively coupled plasma-optical emission spectrophotometer (ICP-OES) for content search of heavy metal after microwave digestion. The heavy metal average concentration in oxidative hair-coloring products was 0.572 ${\mu}g/g$ for Ni, 3.161 ${\mu}g/g$ for Cr, 2.029 ${\mu}g/g$ for Co, 0.420 ${\mu}g/g$ for Cu, respectively. The average of concentration in powder type (henna) was higher than those of other foam and cream type oxidative hair-coloring products as follows; 1.800 ${\mu}g/g$ for Ni, 10.127 ${\mu}g/g$ for Cr, 7.082 ${\mu}g/g$ for Co, 1.451 ${\mu}g/g$ for Cu. Hair coloring products were classified into the six colors - black, dark brown, brown, dark brown, light brown, red brown and analyzed. Brown color had the highest average concentration of Co and the others had the highest average concentration of Cr.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.