• Analytical Science and Technology
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• v.19 no.1
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• pp.107-114
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• 2006

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

• Analytical Science and Technology
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• v.22 no.5
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• pp.395-406
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• 2009

The determination of iodine in the spent nuclear fuel and the volatile behavior during its acid dissolution have been studied by NAA(neutron activation analysis) and electron probe microanalysis (EPMA). Simulated spent fuels (SIMFUELs) were dissolved in $HNO_3$(1+1) at $90^{\circ}C$ for 8 hours. The iodine remained in a dissolver solution after dissolution, and that condensed in dissolution apparatus and trapped in the adsorbent by volatilization during the dissolution were determined, respectively. The condensed iodine was recovered by the redistillation with $HNO_3$(1+1) after transfer of the dissolver solution. The iodines in the dissolver and redistilled solution were separated by solvent extraction followed by ion exchange or precipitation method and determined by RNAA (radiochemical neutron activation analysis). The ion exchange column and filtration kit used for the isolation of iodine, which were prepared with a polyethylene tube, were used as an insert in the pneumatic tube for neutron irradiation. The iodine volatilized during the dissolution of SIMFUELs was collected in a trapping tube containing Ag-silica gel (Ag-impregnated silica gel) adsorbent, and the distribution of iodine trapped in the adsorbents were determined by EPMA. The adsorbing characteristics shown with the SIMFUELs were compared with those shown with a real spent fuel from the nuclear power plant.

• Analytical Science and Technology
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• v.21 no.6
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• pp.510-517
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• 2008

This study has been described the metabolism and excretion in a healthy male urine collected for 26hrs after oral administration of diclofenac. To detect conjugated metabolites of diclofenac, urine sample was acid-hydrolyzed under the conditions of 6M-HCl at over $110^{\circ}C$ for 1hr. During the acidic hydrolysis process, diclofenac and its metabolites were converted into their corresponding lactam-ring through dehydration reaction. As results of chemical conversion by means of hydrolysis, the structures of diclofenac and its metabolites were also changed acidic to basic forms. However, lactam-ring was degraded by hydroxyl ion at basic condition. Thus, the extraction rate of dehydrated diclofenac and its metabolites was not favored at basic condition. For the determination of trace amounts of diclofenac and its metabolites in urine, trimethylsilylation (TMS) with MSTFA was applied and followed by analysis with gas chromatograph-mass spectrometer. In this study, four metabolites that are formed by the hydroxylation of parent drug were mainly detected. Each metabolite was tentatively identified by both interpretation of mass spectra and comparison with previously reported results. In addition, time profile of urinary excretion rate for parent drugs and metabolites was studied. Finally, the metabolic pathway of diclofenac was suggested on the basis of the elucidation of its metabolites and excretion profiles.

• Resources Recycling
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• v.32 no.3
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• pp.3-8
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• 2023

This study discussed production, demand, and future prospects of rubidium, which is an alkali group metal that is highly reactive to various media and requires carefulness in handling, but no significant environmental hazard of rubidium has been reported yet. Rubidium is used in various fields such as optoelectronic equipment, biomedical, and chemical industries. Because of difficulty in production as well as limited demand, the transaction price of rubidium is relatively high, but its detail information such as market status and potential growth is uncertain. However, if the mass production of versatile ultra-high-performance equipment such as quantum computers and the necessity of rubidium use in the equipment are confirmed, there is a possibility that the rubidium market will expand in the future. Rubidium is often found together with lithium, beryllium, and cesium, and may be present in granite containing minerals such as lepidolite and pollucite, as well as in seawater and industrial waste. Several technologies such as acid leaching, roasting, solvent extraction, and adsorption are used to recover rubidium. The maximum recovery efficiency of the rubidium from the sources and the processing above is generally high, but, in many practices, rubidium is not the main recovery target, and therefore the actual recovery effects should depend on presence of other valuable components or impurities, together with recovery costs, energy consumption, environmental issues, etc. In conclusion, although the current production and consumption of rubidium are limited, with consideration of the possible market fluctuations according to the emergence of large-scale demand sources, etc., further investigations by related institutions should be necessary.

• KSCE Journal of Civil and Environmental Engineering Research
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• v.29 no.1A
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• pp.75-84
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• 2009

The present study assesses the chloride threshold level for corrosion of steel in concrete by examining the properties of four different binders used for blended concrete in terms of chloride binding, buffering of cement matrix to a pH fall and the corrosion behaviour. As binders, ordinary Portland cement (OPC), 30% pulverised fuel ash (PFA), 60% ground granulated blast furnace slag (GGBS) and 10% silica fume (SF) were used in a concrete mix. Testing for chloride binding was carried out using the water extraction method, the buffering of cement matrix was assessed by measuring the resistance to an artificial acidification of nitric acid, and the corrosion rate of steel in mortar with chlorides in cast was measured at 28 days using an anodic polarisation technique. Results show that the chloride binding capacity was much affected by $C_{3}A$ content and physical adsorption, and its order was 60% GGBS>30% PFA>OPC>10% SF. The buffering of cement matrix to a pH fall was varied with binder type and given values of the pH. From the result of corrosion test, it was found that the chloride threshold ranged 1.03, 0.65, 0.45 and 0.98% by weight of cement for OPC, 30% PFA, 60% GGBS and 10% SF respectively, assuming that corrosion starts at the corrosion rate of $0.1-0.2{\mu}A/cm^{2}$. The mole ratio of [$Cl^{-}$]:[$H^{+}$], as a new presentation of the chloride threshold, indicated the value of 0.008-0.009, irrespective of binder, which would be indicative of the inhibitive characteristic of binder.

• Journal of the Korean Electrochemical Society
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• v.17 no.2
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• pp.111-118
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• 2014

The electrochemical properties using the cells assembled with the synthesized $LiCoO_2$(LCO) were evaluated in this study. The LCO was synthesized from high-purity cobalt sulfate($CoSO_4$) which is recovered from the cathode scrap in the wastes lithium ion secondary battery(LIB). The leaching process for dissolving the metallic elements from the LCO scrap was controlled by the quantities of the sulfuric acid and hydrogen peroxide. The metal precipitation to remove the impurities was controlled by the pH value using the caustic soda. And also, D2EHPA and $CYANEX^{(R)}272$ were used in the solvent extraction process in order to remove the impurities again. The high-purity $CoSO_4$ solution was recovered by the processes mentioned above. We made the 6 wt.% $CoSO_4$ solution mixed with distilled water. And the 6 wt.% $CoSO_4$ solution was mixed with oxalic acid by the stirring method and dried in oven. $LiCoO_2$ as a cathode material for LIB was formed by the calcination after the drying and synthesis with the $Li_2CO_3$ powder. We assembled the cells using the $LiCoO_2$ powders and evaluated the electrochemical properties. And then, we confirmed possibility of the recyclability about the cathode materials for LIBs.

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.201-210
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• 2017

BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.8
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• pp.1012-1017
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• 2017

Mesembryanthemum crystallinum (Family: Aizoaceae) is an annual plant consisting of ice crystal-shaped bladder cells, which is responsible for its common name ice plant. This study investigated biological activities according to general components and extraction solvent in order to examine the functionality of ice plant. The total content of free amino acids was 32.57 mg/g, including 4.64 mg/g of L-alanine as the most abundant and 2.60 mg/g of ${\gamma}$-aminobutyric acid. Regarding angiotensin converting enzyme inhibitory activities of solvent fractions of ice plant, ethyl acetate fraction and chloroform fraction showed activities of $33.17{\pm}3.20{\sim}88.19{\pm}3.20%$ and $23.72{\pm}2.89{\sim}86.78{\pm}2.24%$, respectively, similar to $Captopril^{(R)}$ ($19.51{\pm}3.44{\sim}84.72{\pm}1.06%$) and $Enalapril^{(R)}$ ($24.93{\pm}1.12{\sim}91.32{\pm}3.62%$) as positive control groups. Regarding inhibition of lipid droplet production in 3T3-L1 preadipocytes by ice plant, anti-adipogenic activities were $53.00{\pm}0.45{\sim}65.75{\pm}0.31%$ and $44.16{\pm}0.29{\sim}63.32{\pm}0.36%$ in the ethyl acetate fraction and butanol fraction, respectively, showing the lowest lipid droplet production. The chloroform fraction and hexane fraction showed activities of $38.33{\pm}0.09{\sim}56.55{\pm}0.50%$ and $31.17{\pm}0.50{\sim}55.10{\pm}1.93%$, respectively, whereas the water fraction showed activity of $26.32{\pm}2.27{\sim}49.48{\pm}0.05%$. Therefore, all solvent fractions inhibited fat accumulation of 3T3-L1 preadipocytes according to treatment concentration. According to the results above, it would be possible to utilize ice plant as a new health functional material.

• 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 Korean Wood Science and Technology
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• v.45 no.5
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• pp.599-612
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• 2017

Human hair (HH) is produced as a waste from beauty parlor and barbershop. HH-based adhesives were formulated with NaOH-hydrolyzed HH, $H_2SO_4$-hydrolyzed chicken blood (CB) and PF as a crosslinking agent. Physicochemical properties and retention rate against hot water of the adhesives were measured to investigate the potential of HH as a raw material of wood adhesives. HH was composed of keratin-type protein of 80% and over. Ash of less than 0.1% was contained in HH. Among the amino acids included in HH, glutamic acid showed the highest content, followed by cysteine, serine, arginine and threonine. Solid content of the adhesives ranged from 33.2% to 41.8% depending on hydrolysis conditions of HH and PF type. Viscosity at $25^{\circ}C$ ranged from 300 to $600mPa{\cdot}s$ resulting in a sprayable adhesive. Retention rate against hot water measured to evaluate the water resistance of adhesives was the highest in the cured resin formulated with 5% NaOH-hydrolyzed HH and 5% $H_2SO_4$-hydrolyzed CB. Meanwhile, the molar ratio of formaldehyde to phenol in PF did not have a significant impact on the retention rate of HH-based adhesives. When the retention rates of HH-based adhesives were compared to those of conventional wood adhesive resins used for the production of wood-based panels extensively, HH-based adhesives formulated with 30 wt% PF showed lower retention rate than commercial urea-formaldehyde resin. However, when PF content was increased to 35 wt%, the retention rate greatly increased and approached to that of commercial melamine-urea-formaldehyde resin. Except for the results mentioned above, the analysis of economic feasibility suggests that HH-based adhesives can be used for the production of wood-based panels if HH is hydrolyzed in proper conditions and then the HH-based adhesives are formulated by the HH hydrolyzates with 35 wt% PF.