• 제목/요약/키워드: Sulfate

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Changes Occurred in Protein and Amino Acid Compositions during Postmortem Aging of White and Dark Muscle of Yellowtail at $2^{\circ}C$ (방어 보통육과 혈합육의 단백질 및 아미노산조성의 사후변화)

  • KIM Chang-Yang;CHOI Yeung-Joon;PYEUN Jae-Hyeung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.15 no.2
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    • pp.123-136
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    • 1982
  • We investigated the changes in protein and free amino acid compositions of the muscles, and amino acid composition of the muscle proteins during postmortem storage of dorsal white and lateral dark muscles of Yellowtail, Seriola quinqueradita, which were kept at $2^{\circ}C$. We present an extensive discussion on the relationship between the changes of freshness and those of protein compositions in the white and the dark muscle of the red-fleshed fish by analyzing polyacrylamide gel electrophoretograms of $NaDodSO_4-solubilized$ sarcoplasmic and myofibrillar proteins extracted from the both muscles. By assessing K-value, total volatile basic nitrogen and pH value as a criterion of freshness, we found that the dark muscle undergoes a more rapid decrease in its freshness compared to that of the white muscle. The contents of the sarcoplasmic and the myofibrillar protein were decreased with postmortem aging of the muscles while those of the residual intracellular protein were increased, and these changes were somewhat faster in the dark muscle than in the white muscle. From the analysis of the electrophoretograms and their densitograms, we found that the sarcoplasmic proteins of the white and the dark muscle were respectively composed of 16 and 12 components. The sarcoplasmic protein of the white muscle lapsed for 10 days showed an increase of 18,000 and 41,000 dalton components, and a gradual decrease of 23,000 and 23,500 dalton components, whereas the sarcoplasmic protein of the dark muscle lapsed for 9 days showed a decrease of 49,000 dalton component, an appearence of a newly formed component of 47,000 dalton, and a disappearance of 26,000 dalton component. The electrophoretograms of the myofibrillar proteins shelved that the white and the dark muscle were composed of 17 and 16 components, respectively. Depending on the lapsed time of postmortem under the controlled condition, the myofibrillar proteins of the white muscle showed an increase of 40,000 dalton component, a gradual decrease of 37,500 dalton component, an appearance of a newly forming component of 32,000 dalton and a disappearance of 26,000 dalton component. On the other hand, the myofibrillar proteins of the dark muscle showed an increase of 58,000 and 64,000 dalton bands, a disappearance of light chain-2 protein and an appearance of a newly forming protein of 32,000 dalton. These changes on the electrophoretic patterns in the dark muscle were more rapid than those in the white muscle. In almost all of the cases, we observed that the changes in the sarcoplasmic protein were faster than those in the myofibrillar protein. The analysis of amino acid of the both muscle proteins showed that the white muscle was rich in glutamic acid, aspartic acid, leucine, arginine, lysine, etc. but was poor in proline and tryptophan. No significant difference was found in the amino acid composition of protein of both the white and the dark muscles. The sample of white muscle lapsed for 10 days shows a remarkable decrease in glutamic and aspartic acids, while that of the dark muscle lapsed for 9 days shows an appreciable decrease in alanine, glycine and arginine. The free amino acid compositions of the white and the dark muscles are respectively characterized with $63\%$ of histidine and $67\%$ of taurine with respect to the total free amino acids of the yellowtail at-death, respectively. The white muscle lapsed for 10 days showed an increase of histidine, valine and taurine, and a slight decrease of alanine, leucine and glycine. The dark muscle lapsed for 9 days shelved an increase of taurine, phenylalanine and glycine, and a decrease of histidine, alanine and serine.

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[ $Gd(DTPA)^{2-}$ ]-enhanced, and Quantitative MR Imaging in Articular Cartilage (관절연골의 $Gd(DTPA)^{2-}$-조영증강 및 정량적 자기공명영상에 대한 실험적 연구)

  • Eun Choong-Ki;Lee Yeong-Joon;Park Auh-Whan;Park Yeong-Mi;Bae Jae-Ik;Ryu Ji Hwa;Baik Dae-Il;Jung Soo-Jin;Lee Seon-Joo
    • Investigative Magnetic Resonance Imaging
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    • v.8 no.2
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    • pp.100-108
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    • 2004
  • Purpose : Early degeneration of articular cartilage is accompanied by a loss of glycosaminoglycan (GAG) and the consequent change of the integrity. The purpose of this study was to biochemically quantify the loss of GAG, and to evaluate the $Gd(DTPA)^{2-}$-enhanced, and T1, T2, rho relaxation map for detection of the early degeneration of cartilage. Materials and Methods : A cartilage-bone block in size of $8mm\;\times\;10mm$ was acquired from the patella in each of three pigs. Quantitative analysis of GAG of cartilage was performed at spectrophotometry by use of dimethylmethylene blue. Each of cartilage blocks was cultured in one of three different media: two different culture media (0.2 mg/ml trypsin solution, 1mM Gd $(DTPA)^{2-}$ mixed trypsin solution) and the control media (phosphate buffered saline (PBS)). The cartilage blocks were cultured for 5 hrs, during which MR images of the blocks were obtained at one hour interval (0 hr, 1 hr, 2 hr, 3 hr, 4 hr, 5 hr). And then, additional culture was done for 24 hrs and 48 hrs. Both T1-weighted image (TR/TE, 450/22 ms), and mixed-echo sequence (TR/TE, 760/21-168ms; 8 echoes) were obtained at all times using field of view 50 mm, slice thickness 2 mm, and matrix $256\times512$. The MRI data were analyzed with pixel-by-pixel comparisons. The cultured cartilage-bone blocks were microscopically observed using hematoxylin & eosin, toluidine blue, alcian blue, and trichrome stains. Results : At quantitation analysis, GAG concentration in the culture solutions was proportional to the culture durations. The T1-signal of the cartilage-bone block cultured in the $Gd(DTPA)^{2-}$ mixed solution was significantly higher ($42\%$ in average, p<0.05) than that of the cartilage-bone block cultured in the trypsin solution alone. The T1, T2, rho relaxation times of cultured tissue were not significantly correlated with culture duration (p>0.05). However the focal increase in T1 relaxation time at superficial and transitional layers of cartilage was seen in $Gd(DTPA)^{2-}$ mixed culture. Toluidine blue and alcian blue stains revealed multiple defects in whole thickness of the cartilage cultured in trypsin media. Conclusion : The quantitative analysis showed gradual loss of GAG proportional to the culture duration. Microimagings of cartilage with $Gd(DTPA)^{2-}$-enhancement, relaxation maps were available by pixel size of $97.9\times195\;{\mu}m$. Loss of GAG over time better demonstrated with $Gd(DTPA)^{2-}$-enhanced images than with T1, T2, rho relaxation maps. Therefore $Gd(DTPA)^{2-}$-enhanced T1-weighted image is superior for detection of early degeneration of cartilage.

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The Hardness Water Production By RO/NF/ED Linking Process From Deep Seawater (RO/NF/ED 연계 공정에 의한 고경도 담수 제조)

  • Moon, Deok-Soo;Kim, Kwang Soo;Gi, Ho;Choi, Mi Yeon;Jung, Hyun Ji;Kim, Hyun Ju
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.16 no.4
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    • pp.227-238
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    • 2013
  • The purpose of this study is to develop a process technology to produce high hardness drinking water which meet drinking water standard, remaining useful minerals like magnesium and calcium in the seawater desalination process while removing the sulfate ions and chloride ions. Seawater have been separated the concentrated seawater and desalted seawater by passing on Reverse Osmosis membrane (RO). Using Nano-filtration membrane (NF), We were prepared primary mineral concentrated water that sodium chloride were not removed. By the operation of electro-dialysis (ED) having ion exchange membrane, we were prepared concentrated mineral water (Mineral enriched desalted water) which the sodium chloride is removed. We have produced the high hardness water to meet the drinking water quality standards by diluting the mineral enriched desalted water with deionized water by RO. Reverse osmosis membranes (RO) can separate dissolved material and freshwater from seawater (deep seawater). The desalination water throughout the second reverse osmosis membrane was completely removed dissolved substances, which dissolved components was removed more than 99.9%, its the hardness concentration was 1 mg/L or less and its chloride concentration was 2.3 mg/L. Since the nano-filtration membrane pore size is $10^{-9}$ m, 50% of magnesium ions and calcium ions can not pass through the nano-filtration membrane, while more than 95% of sodium ions and chloride ions can pass through NF membrane. Nano-filtration membrane could be separated salt components like sodium ion and chloride ions and hardness ingredients like magnesium ions and calcium ions, but their separation was not perfect. Electric dialysis membrane system can be separated single charged ions (like sodium and chloride ions) and double charged ions (like magnesium and calcium ions) depending on its electrical conductivity. Above electrical conductivity 20mS/cm, hardness components (like magnesium and calcium ions) did not removed, on the other hand salt ingredients like sodium and chloride ions was removed continuously. Thus, we were able to concentrate hardness components (like magnesium and calcium ions) using nano-filtration membrane, also could be separated salts ingredients from the hardness concentration water using electrical dialysis membrane system. Finally, we were able to produce a highly concentrated mineral water removed chloride ions, which hardness concentration was 12,600 mg/L and chloride concentration was 2,446 mg/L. By diluting 10 times these high mineral water with secondary RO (Reverse Osmosis) desalination water, we could produce high mineral water suitable for drinking water standards, which chloride concentration was 244 mg/L at the same time hardness concentration 1,260 mg/L. Using the linked process with reverse osmosis (RO)/nano filteration (NF)/electric dialysis (ED), it could be concentrated hardness components like magnesium ions and calcium ions while at the same time removing salt ingredients like chloride ions and sodium ion without heating seawater. Thus, using only membrane as RO, NF and ED without heating seawater, it was possible to produce drinking water containing high hardness suitable for drinking water standard while reducing the energy required to evaporation.

Studies on the Cellulase produced by Myriococcum of albomyces (Myriococcum albomyces가 생산하는 Cellulase에 관한 연구)

  • Chung, Dong-Hyo
    • Applied Biological Chemistry
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    • v.14 no.1
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    • pp.59-97
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    • 1971
  • As a study on the cellulase of Myriococcum albomyces the culture media for enzyme formation and properties of its crude preparation were investigated and the crude enzyme preparation was further fractionated. The results are summarized as follows: 1. Wheat bran solid culture produced stronger activities of cellulase than rice bran or defatted soy bean meal solid culture. 2. Shaking culture with wheat bran, rice bran or defatted soy bean meal produced higher cellulase activities than solid culture with the corresponding media. 3. The enzyme formation was higher at $45^{\circ}C$ than at $37^{\circ}C$ or $50^{\circ}C$ regardless of the kind of culture medium. 4. The formation of CMCase activity was more promoted by organic nitrogen source than inorganic nitrogen source. 5. The formation of cellulase activities were increased 1.5 to 3.0-fold by adding CMC, Avicel or cellulose powder as an inducer into 5% wheat bran basal medium. 6. Cellulase production using a tank culture procedure with addition of CMC or Avicel as an inducer was the highest at fifth day and thereafter decreased slightly. 7. The crude enzyme preparation showed pH optimum in 4.0 to 4.5, and pH stability in the range of 3.5 to 8.0. Optimum temperature for the activity was $65^{\circ}C$ which was higher than among other cellulases and it was stable at $60^{\circ}C$ for 120 minutes. 8. Dialyzed crude enzyme was activated by $Ca^{++}$ and $Mg^{++}$, but inhibited by $Hg^{++}$, $Cu^{++}$ and $Ag^{+}$. 9. Four different types of cellulase, i. e., fraction I, fraction II-a, fraction II-b, and fraction III were purified from the culture filtrate of Myriococcum albomyces through a sequence of ammonium sulfate fractionation, and elution chromatography on DEAE-Sephadex A-25, Amberlite CG-25 type 2 and hydroxyapatite columns. 10. These four cellulase fractions were showed to be homogenous by electrophoresis and ultracentrifugation and also gave a typical ultraviolet absorption spectrum of protein. 11. Four purified fraction showed different specificity toward substrates, fraction I has a stronger activity toward Avicel, cellulose powder, and gauze than that of other cellulase fractions. Fraction II-a had a powerful activity toward cellobiose but it was almost inactive agaisnt fibrous cellulose contrary to fraction I. On the contrary, the main component fraction II-b had a fairly higher activity on CMC and Avicel. Activity of fraction II-b toward cellobiose was about one-third of that of fraction II-a and activity on Avicel was lower than that of fraction I. Fraction III had a more powerful activity in decreasing viscosity of CMC. 12. Final hydrolysis products of fibrous cellulose by each fraction were cellobiose and glucose. Whereas oligosaccharides were predominant in the early stage of hydrolysis, prolonged reaction produced more glucose than cellobiose. Fraction I and fraction II-a acted synergically on Avicel. 13. Optimum pH for the activities of cellulase fraction I, fraction II-a, fraction II-b and fraction III were found to be 5.5, 5.0, 4.0 and $4.0{\sim}4.5$, respectively. These fractions were found to be stable in the range of pH $3.0{\sim}7.5$. 14. Optimum temperature for the activities of fraction I, fraction II-a, fraction II-b, and fraction III were $50^{\circ}C$, $55^{\circ}C$, $60^{\circ}C$ and $55^{\circ}C$, respectively. No less of activity was found by heating 120 minutes at $55^{\circ}C$ and fraction II-a was more stable than the others at $60^{\circ}C$. 15. Fraction I and fraction II-b were activated by $Ca^{++}$ and $Mg^{++}$ but inhibited by $Hg^{++}$ and $Ag^{+}$.

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Studies on the Induction of Available Mutants of Takju Yeast by UV light Irradiation (part 2) -On the Physiological Characteristics of the Mutants- (자외선조사(紫外線照射)에 의한 탁주효모(酵母)의 변이주육성(變異株育成)에 관한 연구 (제 2 보) -변이주(變異株)의 생리적성질(生理的性質)에 관하여)

  • Kim, Chan-Jo;Oh, Man-Jin;Kim, Seung-Yul
    • Applied Biological Chemistry
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    • v.18 no.1
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    • pp.16-22
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    • 1975
  • This experiment was carried out to investigate the physiological characteristics of two original yeasts, 5-Y-5 and 6-Y-6, which selected from 24 Takju yeasts and three mutants, 30-24,30-81 and 40-27. induced from two original yeasts by the irradiation of UV light. The results were summarized as follows. 1) Alcohol tolerances of three mutants were decreased in some degree as compared with those of original yeasts. 2) Tolerances of lactic and citric acids of acid producing mutant 30-81, was increased than those of original yeasts. 3) In the case of using ammonium sulfate as a nitrogen source, two original yeasts and three mutants required Ca-pantothenate as a essential growth factor and four strains of yeasts except the mutant, 30-81, required biotin as a stimulated growth factor, When asparagine was used as a nitrogen source, two original yeasts and three mutants showed the same as above result but the stimulated effect of biotin was far less. 4) Propagation powers of the mutants were weaken than those of original yeasts, particular that of acid producing mutant, 30-81, was the weakest in the three mutants. 5) The optimum temperature for fermentation of original yeasts were $30^{\circ}C\;to\;35^{\circ}C$ but three mutants were $25^{\circ}C\;to\;30^{\circ}C$. 6) The optimum pH for fermentation of original yeasts were pH 5 to 6, and there is no appreciable difference between original yeasts and three mutants. The fermentation power of mutant,30-81, was decreased more rapidly than those of other mutants according to approach neutral. Three mutants were more sensible to heat than original yeasts. 7) Two original yeasts and three mutants were inhibited more over 20 percent of sugar for fermentation and three mutants were more sensible to sugar concentration than original yeasts.

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Hydrochemical and Isotopic Characteristics, and Origin of Noble Gas for Low-temperature Hot Spring Waters in the Honam Area (호남지역 저온형 온천수의 수리지화학적 및 안정동위원소 특성과 영족기체의 기원에 관한 연구)

  • Jeong, Chan-Ho;Hur, Hyun-Sung;Nagao, Keisuke;Kim, Kyu-Han
    • Economic and Environmental Geology
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    • v.40 no.5
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    • pp.635-649
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    • 2007
  • Geochemical composition, stable isotopes $({\delta}^{18}O,\;{\delta}D,\;{\delta}^{34}S)$ and noble gases(He, Ne and Ar) of nine hot spring water and three groundwater for five hot springs(Jukam, Hwasun, Dokog, Jirisan, Beunsan) from the Honam area were analyzed to investigate the hydrogeochemical characteristics and the hydrogeochemical evolution of the hot spring waters, and to interpret the source of sulfur, helium and argon dissolved in the hot spring waters. The hot spring waters show low water temperature ranging from 23.0 to $30.5^{\circ}C$ and alkaline characteristics of pH 7.67 to 9.98. Electrical conductivity of hot spring waters is $153{\sim}746{\mu}S/cm$. Groundwaters in this area were characterized by the acidic to neutral pH range$(5.85{\sim}7.21)$, the wide electrical conductivity range $(44{\sim}165{\mu}S/cm)$. The geochemical compositions of hot spring and groundwaters can be divided into three water types: (1) $Na-HCO_3$ water type, (2) Na-Cl water type and (3) $Ca-HCO_3$ water type. The hot spring water of $Ca-HCO_3$ water type in early stage have been evolved through $Ca(Na)-HCO_3$ water type into $Na-HCO_3$ type in final stage. In particular, Jurim alkaline(pH 9.98) hot spring water plotted at the end point of $Na-HCO_3$ type in the Piper diagram is likely to arrive into the final stage in geochemical evolution process. Hydrogen and oxygen isotopic data of the hot spring water samples indicate that the hot spring waters originated from the local meteoric water showing latitude and altitude effects. The ${\delta}^{34}S$ value for sulfate of the hot spring waters varies widely from 0.5 to $25.9%o$. The sulfur source of most hot spring waters in this area is igneous origin. However, The ${\delta}^{34}S$ also indicates the sulfur of JR1 hot water is originated from marine sulfur which might be derived ken ancient seawater sulfates. The $^3He/^4He\;and\;^4He/^{20}Ne$ ratios of the hot spring waters range from $0.0143{\times}10^{-6}\;to\;0.407{\times}10^{-6}\;and\;6.49{\sim}584{\times}10^{-6}$, respectively. The hot spring waters are plotted on the mixing line between air and crustal components. It means that the He gas in the hot spring waters was mainly originated from crustal sources. However, the JR1 hot spring water show a little mixing ratio of the helium gas of mantle source. The $^{40}Ar/^{36}Ar$ ratios of hot spring water are in the range from $292.3{\times}10^{-6}\;to\;304.1{\times}10^{-6}$, implying the atmospheric argon source.

Mineralogy and Geochemistry of the Jeonheung and Oksan Pb-Zn-Cu Deposits, Euiseong Area (의성(義城)지역 전흥(田興) 및 옥산(玉山) 열수(熱水) 연(鉛)-아연(亞鉛)-동(銅) 광상(鑛床)에 관한 광물학적(鑛物學的)·지화학적(地化學的) 연구(硏究))

  • Choi, Seon-Gyu;Lee, Jae-Ho;Yun, Seong-Taek;So, Chil-Sup
    • Economic and Environmental Geology
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    • v.25 no.4
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    • pp.417-433
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    • 1992
  • Lead-zinc-copper deposits of the Jeonheung and the Oksan mines around Euiseong area occur as hydrothermal quartz and calcite veins that crosscut Cretaceous sedimentary rocks of the Gyeongsang Basin. The mineralization occurred in three distinct stages (I, II, and III): (I) quartz-sulfides-sulfosalts-hematite mineralization stage; (II) barren quartz-fluorite stage; and (III) barren calcite stage. Stage I ore minerals comprise pyrite, chalcopyrite, sphalerite, galena and Pb-Ag-Bi-Sb sulfosalts. Mineralogies of the two mines are different, and arsenopyrite, pyrrhotite, tetrahedrite and iron-rich (up to 21 mole % FeS) sphalerite are restricted to the Oksan mine. A K-Ar radiometric dating for sericite indicates that the Pb-Zn-Cu deposits of the Euiseong area were formed during late Cretaceous age ($62.3{\pm}2.8Ma$), likely associated with a subvolcanic activity related to the volcanic complex in the nearby Geumseongsan Caldera and the ubiquitous felsite dykes. Stage I mineralization occurred at temperatures between > $380^{\circ}C$ and $240^{\circ}C$ from fluids with salinities between 6.3 and 0.7 equiv. wt. % NaCl. The chalcopyrite deposition occurred mostly at higher temperatures of > $300^{\circ}C$. Fluid inclusion data indicate that the Pb-Zn-Cu ore mineralization resulted from a complex history of boiling, cooling and dilution of ore fluids. The mineralization at Jeonheung resulted mainly from cooling and dilution by an influx of cooler meteoric waters, whereas the mineralization at Oksan was largely due to fluid boiling. Evidence of fluid boiling suggests that pressures decreased from about 210 bars to 80 bars. This corresponds to a depth of about 900 m in a hydrothermal system that changed from lithostatic (closed) toward hydrostatic (open) conditions. Sulfur isotope compositions of sulfide minerals (${\delta}^{34}S=2.9{\sim}9.6$ per mil) indicate that the ${\delta}^{34}S_{{\Sigma}S}$ value of ore fluids was ${\approx}8.6$ per mil. This ${\delta}^{34}S_{{\Sigma}S}$ value is likely consistent with an igneous sulfur mixed with sulfates (?) in surrounding sedimentary rocks. Measured and calculated hydrogen and oxygen isotope values of ore-forming fluids suggest meteoric water dominance, approaching unexchanged meteoric water values. Equilibrium thermodynamic interpretation indicates that the temperature versus $fs_2$ variation of stage I ore fluids differed between the two mines as follows: the $fs_2$ of ore fluids at Jeonheung changed with decreasing temperature constantly near the pyrite-hematite-magnetite sulfidation curve, whereas those at Oksan changed from the pyrite-pyrrhotite sulfidation state towards the pyrite-hematite-magnetite state. The shift in minerals precipitated during stage I also reflects a concomitant $fo_2$ increase, probably due to mixing of ore fluids with cooler, more oxidizing meteoric waters. Thermodynamic consideration of copper solubility suggests that the ore-forming fluids cooled through boiling at Oksan and mixing with less-evolved meteoric waters at Jeonheung, and that this cooling was the main cause of copper deposition through destabilization of copper chloride complexes.

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Studies on the fate of nitrogen in the paddy soil (답토양(沓土壤)에서 질소(窒素)의 동태(動態)에 관(關)한 연구(硏究))

  • Kim, Kwang Sik
    • Korean Journal of Soil Science and Fertilizer
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    • v.9 no.1
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    • pp.17-23
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    • 1976
  • In order to investigate the fate of nitrogen in the paddy soil, Suchang, Hwasoon and Susan soil which have different properties, were treated with several nitrogen fertilizers such as ammonium chloride, ammonium sulfate, urea and SCU (sulfur-coated urea), and incubated under water-logged condition in $30^{\circ}C$ incubator. $NH_4-N$, $NO_3-N$, $Fe^{++}$ and pH in soil and stagnant water, were determined at 10, 20, 30, 40 and 50 days after incubation. The obtained results were summarized as follows: 1. The effect of rising temperature was increased in order of Hwasoon>Suchang>Susan and the effect of air drying soil was risen in order of Susan>Hwasoon>Suchang, while the rate of ammonication was in order of Susan>Suchang>Hwasoon. 2. The changes of $NH_4-N$ in stagnant water was dependent upon the nitrogen concentration of $NH_4Cl$ and $(NH_4)SO_4$ plat was high and decreased after 30 days incubation, but increased after 40 days and then decreased again. In contrast with the above, $NH_4-N$ concentration of urea and SCU plot was low but the change showed slightly through the incubation period. 3. Accumulation of $NH_4-N$ in the oxidative layer of the $NH_4Cl$ and $(NH_4)_2SO_4$ plot was higher than that of urea and SCU plot and $NH_4-N$ content was decreased with the incubation period. The change of $NH_4-N$ in the reductive layer showed the same pattern. 4. The changes of $NO_3-N$ in the stagnant water were different according to soil properties and nitrogen fertilizer. $NO_3-N$ concentration in stagnant water of urea and SCU plot was higher than in the $NH_4-Cl$ $(NH_4)_2SO_4$ plot and nearly disappeared after 30 to 40 days incubation. 5. The $NO_3-N$ concentration in the oxidative layer of soil was higher than reductive layer. The pattern of change was different in accordance with soil properties and nitrogen fertilizers. In general, nitrification in urea and SCU plot was more increased than $(NH_4)_2SO_4$ plot. In reductive layer, the concentration of $NO_3-N$ was very low until 30 days incubation and thereafter increased slightly. 6. Upon the concentration of $NH_4-N$ and $NO_3-N$ in stagnant water and soil, it was assumed that denitification of urea and SCU plot was higher than $NH_4Cl$ and $(NH_4)_2SO_4$ plot and denitrified nitrogen in incubation period was above 50%.

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Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • 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.

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.