• KSBB Journal
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• v.14 no.3
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• pp.384-388
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• 1999

We have used high pH anion-exchange chromatography to analyze low level (below $20{\mu}M$) $\alpha$-D-glucose-1-phosphate (G-1-P) that can be used as a cytostatic compound, an antibiotic, and immunosuppressive drug. Our chromatographic method afforded excellent peak resolution and seletivity for glucose-6-phosphate and various maltooligosaccharides as well as G-1-P. The pulsed amperometric detector yielded linear response on G-1-P ranging from 2 - $20{\mu}M$, giving slope of $4.8{\times}10^4$(peak area/${\mu}M$). The detection limit was $2{\mu}M$. This method was applied to the purification of thermophilic $\alpha$-glucan phosphorylase from Thermus caldophilus. The technique will be extremely useful in future studies concerning carbohydrate metabolism in living organisms.

• Analytical Science and Technology
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• v.20 no.4
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• pp.308-314
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• 2007

The analytical method of HPLC with the radial-flow electrochemical cell (RFEC) has been developed to determine doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin simultaneously by employing a reversed-phase chromatography. Anthracyclines were detected at -0.74 V vs. a Ag/AgCl (0.01 M NaCl) reference electrode, a potential of diffusion current plateau in the mobile phase. At a $V_f$ of 1.0 mL/min doxorubicin, epirubicin, daunorubicin and idarubicin appeared at a retention time ($t_r$) of 6.4 min, 7.4 min, 12.7 min and 18.4 min, respectively, while at a $V_f$ of 0.6 mL/min, doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin appeared at a $t_r$ of 9.9 min, 11.5 min, 13.5 min, 19.6 min and 28.7 min, respectively. The linearity between each anthracycline injected ($2.40{\times}10^{-7}M{\sim}1.42{\times}10^{-5}M$) and peak area (charge) was excellent with the square of the correlation coefficient ($R^2$) higher than 0.999. The detection limits were $1.0{\times}10^{-8}M{\sim}1.5{\times}10^{-7}M$ for the five anthracyclines. Within-day precision for the five anthracyclines were in reasonable relative standard deviations less than 3 % ($1.00{\times}10^{-6}M{\sim}1.42{\times}10^{-5}M$) except the lower concentrations less than $0.7{\mu}M$. Solid phase extractions of $1.00{\times}10^{-5}M$ epirubicin, $0.48{\times}10^{-5}M$ nogalamycin and $1.52{\times}10^{-5}M$ daunorubicin from human serum with a $C_{18}$ cartridge resulted in 97 %, 100 % and 90 % of recoveries, respectively.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.68-74
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• 2017

An analytical method for detecting metamifop residue in paddy water, soil, and rice with high performance liquid chromatography (HPLC) was developed. Water was extracted with ethyl acetate before analyzing by HPLC. Soil residues were extracted with acetone under acidic condition and after purifying with $Extrelut^{(R)}$ NT, and silica SPE, the residue was analyzed by HPLC. For residue analysis in rice, the procedure involved extraction with acetone, purification with $Extrelut^{(R)}$ NT, partitioning between acetonitrile/hexane, purification with silica SPE cartridge, and analysis by HPLC. The limit of detection (LOD) was 1.0 ng, limit of quantitation (LOQ) was 3.0 ng, and method limit of quantitation (MLOQ) were 0.001 mg/L for paddy water, 0.01 mg/kg for rice and soil, respectively. Standard calibration curve shows linearity from 0.05 mg/kg to 5.0 mg/kg ($R^2=0.9999$). The recoveries in fortified paddy water were $91.3{\pm}3.5%$ (0.01 mg/L level) and $93.2{\pm}6.3%$ (0.05 mg/L level). The recoveries in fortified paddy soils were $92.5{\pm}4.0%$ (0.1 mg/kg level) and $92.7{\pm}4.0%$ (0.5 mg/kg level) in soil A, while, $102.3{\pm}4.4%$ (0.1 mg/kg level) and $98.9{\pm}7.9%$ (0.5 mg/kg level) in soil B, respectively. The recoveries in fortified rice were $93.0{\pm}6.9%$ (0.1 mg/kg level) and $85.0{\pm}3.5%$ (0.5 mg/kg level). This method was proved to be effective and can be used to determine the metamifop residue in paddy water, paddy soil, and rice.

• Journal of the Mineralogical Society of Korea
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• v.28 no.3
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• pp.245-253
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• 2015

The performance of $TiO_2$ photo-catalytic oxidation process is significantly dependent on the amount of hydroxyl radicals produced during the process, and it is an essential prerequisite to quantify its production. However, precise and accurate methods for quantification of hydroxyl radicals have not been developed so far. For this reason, this study was initiated to compare existing methods for analysis of hydroxyl radicals produced by $TiO_2$ photo-catalytic oxidation and to propose a new method to overcome the limitation of established methods. To simulate $TiO_2$ photo-catalytic oxidation process, Degussa P25 which has been widely used as a standard $TiO_2$ photo-catalyst was used with the dose of 0.05 g/L. The light source of process was UVC mercury low-pressure lamp (11 W, $2,975mW/cm^2$). The results indicate that both potassium iodide (KI)/UV-vis spectrometer and terephthalic acid (TPA)/fluorescence spectrometer methods could be applied to qualitatively measure hydroxyl radicals via detection of triiodide ion ($I_3{^-}$) and 2-hydroxyterephthalic acid which are produced by reactions of iodine ion ($I^-$) and TPA with hydroxyl radicals, respectively. However, it was possible to quantitatively measure hydroxyl radicals using TPA method coupled with high-performance liquid chromatograph (HPLC). The analytical results using TPA/HPLC method show that hydroxyl radical of 0.013 M was produced after 8 hours operation of photo-catalytic oxidation under specific experimental conditions of this study. The proposed method is expected to contribute to precise the evaluation of the performance of photo-catalytic oxidation process.

• Tuberculosis and Respiratory Diseases
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• v.50 no.2
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• pp.158-170
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• 2001

Background : Although an oxidants and antioxidants imbalance has been considered in the pathogenesis of chronic obstructive pulmonary disease (COPD), there is a paucity of reports focussing on the smoking-induced changes of oxidants and antioxidants in COPD. Method : The concentration of antioxidants (ascorbic acid, uric acid, retinol, and $\alpha$- & $\gamma$-tocopherol) was measured in the serum and induced sputum of 30 healthy controls and 34 stable COPD patients using high performance liquid chromatography (HPLC). The inhibition of lipid peroxidation as an index of antioxidant capacity was measured in the serum by a TBA assay. Results : The serum concentration of ascorbic acid, $\alpha$-tocopherol, and retinol were significantly lower in the patients with COPD than in healthy controls ($484.8{\pm}473.3$ vs $1497.8{\pm}819.2\;pmol/L$, $48.38{\pm}17.34$ vs $73.96{\pm}26.29\;pmol/L$, p<0.001, and $9.51{\pm}8.33$ vs $15.01{\pm}5.88\;pmol/L$, p<0.05, respectively, mean$\pm$SD). However, there were little differences in the ascorbic acid and uric acid concentrations in the induced sputum between the COPD patients and the controls. The induced sputum to serum ratio of ascorbic acid was significantly higher in COPD patients compared with healthy control (0.375 vs 0.085, p<0.05). In the normal controls, the serum ascorbic acid concentration was lower in smokers than in nonsmokers ($1073{\pm}536$ vs $1757{\pm}845\;pmol/L$, p<0.05), but the level was still higher than that of the COPD patients (p<0.05). The serum retinol levels were correlated with $FEV_1$ in COPD patients (r=0.58, p<0.05). The products of lipid peroxidation were increased in normal smokers and COPD compared with norma1 nonsmokers ($115.56{\pm}19.93$ vs $120.02{\pm}24.56$ vs $91.87{\pm}20.71\;{\mu}mol/{\mu}mol$ Pi of liposome, p<0.05). Conclusion : Cigarette smoking may induce the dep1etion of serum antioxidants and this depletion of antioxidants is suggested to play a role in the pathogenesis of COPD.