• Title/Summary/Keyword: Eluate

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A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants(III) : On-Line System for Preconcentration and Separation of Trace Phenols by HPLC (환경 오염물질의 정량법 개발과 거동에 관한 연구(III) : 미량 페놀류의 HPLC 정량을 위한 온 라인 농축)

  • Lee, Dai Woon;Kim, Jin Young;Park, Young Hun;Moon, Myeong Hee
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.33-39
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    • 1994
  • The purpose on this study was to develop a new improved chromatographic method for determination of trace phenols from environmental waste water. The research was carried out with selected 8 phenols, and solid-phase extraction was employed as sample pretreatment method. The coupling of XAD-4 and Dowex $1{\times}8$ resin as preconcentration column increased the selectivities toward interferences coexisted in matrix. Automation was accomplished with on-line process of pretreatment and HPLC system. After elution of sample through XAD-4 column, phenols were adsorbed by dispersion force, then displaced from it by ACN basified, simultaneously and selectively readsorbed via anion exchange on Dowex $1{\times}8$. Dowex $1{\times}8$ column was washed by water. Phenols readsorbed were removed from Dowex $1{\times}8$ column by a minimum volumn of methanol containing HCl. Each pretreatment step was connected by switching valves and the eluate was directly on-line injected to obtain fast and reliable results into the HPLC. Recovery of phenols was greater than 90%. To examine utility of this method, analysis of phenols from laboratory waste water sample which was added some organic pollutants to find with phenols on environmental waste water were also accomplished without their interference effects.

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Residue Determination of Chlorothalonil in Sesame and Soil (Chlorothalonil의 참깨 및 토양중 잔류소장에 관한 연구)

  • Lee, Kang-Bong;Cho, Ill-Kyu;Shim, Jae-Han;Suh, Yong-Tack
    • Korean Journal of Environmental Agriculture
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    • v.9 no.1
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    • pp.15-22
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    • 1990
  • The efects of application time on the persistence of chlorothalonil in sesame plants and its persistence in soil were studied in the field. A procedure was used which permited the analysis of residues of Chlorothalonil (DACONIL 2787) in sesame(Sesamum indicum L.)and soil. The procedure was based on the multiresidue analytical method using an polarized acetonitrile solution or acidified acetone as the extracting solvent. The DACONIL 2787 is separated from the fat in the extracts by using an activated alumina and Florisil chromatogaphic column. Residues of DACONIL 2787 were determined by subjecting the alternate eluate from the Florisil column to gas chromatographic analysis(ECD). Residue of chlorothalonil in sesame are proved to 0.06 ppm for six sprays, 3rd day before harvest The half-life of chlorothalonil in soil proved to be 8.9 days and residues of chlorothalonil was only 0.03 ppm 100 days after application of 15 ppm.

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Studies on $\alpha$-Amylase of Bacillus circulans F-2 (Part I) Purification of $\alpha$-amylase (Bacillus circulans F-2가 생산하는 $\alpha$-Amylase에 관한 연구 (제 1보) $\alpha$-Amylase의 정제)

  • ;Hajime Taniguchi;Yoshiharu Maruyama
    • Microbiology and Biotechnology Letters
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    • v.9 no.4
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    • pp.185-190
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    • 1981
  • 1. $\alpha$-amylase from B. circulans F-2 was purified with specific activity 55.0 u/mg. protein (about 23 times of the original specific activity) and the yield of 25.5%, by means of corn starch absorption, salting out with ammonium sulfate (80% saturation), gel filtration on Bio-Gel P-100 and DE-32 column chromatography. 2 The purified enzyme showed two closely migrated protin bands on polyacrylamide disc gel electrophoresis, both of which have amylase activity judging from the activity staining of the gel. On SDS-polyacrylamide disc gel electrophoresis, however, the purified enzyme showed a single band suggesting that those two bands are the charge isomers of an amlyase having the slightly different charge. 3. Plot of log mobility of two bands versus polyacrylamide gel concentration according to Hedrick and Smith gave the parallel lines indicating them to be charge isomers. 4. To confirm the action pattern of two enzyme protein bands, each band was separated and was eluted from the gel and eluates were incubated with soluble starch. Oligosaccharide pattern produced by each eluate was examined by paper chromatography. The eluates of two bands showed the same action pattern. 5. The maltohexaose was the only hydrolysis product of soluble starch in the early stage of hydrolysis.

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A Study on the Separation of Neodymium from the Simulated Solution of $U_3Si/Al$ Spent Nuclear Fuel (모의 사용후분산핵연료($U_3Si/Al$) 용해용액으로부터 네오디뮴 분리에 관한 연구)

  • Choi, Kwang Soon;Kim, Jung Suk;Han, Sun Ho;Park, Soon Dal;Park, Yeong Jae;Joe, Kih Soo;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.584-591
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    • 2000
  • The separation of Nd from the simulated $U_3Si/Al$ spent fuel solution with sequential two-step anion exchange separation has been studied. To prepare the simulated $U_3Si/Al$ spent nuclear fuel, unirradiated $U_3Si/Al$ whose composition consists of small $U_3Si$ particle dispersed in an Al matrix with Al cladding was dissolved with a mixture of 4 M HCl and 10 M $HNO_3$ and 8 or 15 fission product elements were added to the dissolved solution. The trace amount of silica in the solutions was removed by evaporating to dryness with HF and the U was adsorbed on the first anion exchange resin. Neodymium can be purely isolated from the fission product elements with a methanol-nitric acid eluent using the second anion exchange resin. A large excess of Al didn't influence on the elution velocity of Nd, but reduced the eluted contents of Nd, Al, Eu, Gd, Sm and Sr, A large amount of Al was removed first from the column with 3 mL of loading solution (0.8 M $HNO_3$/99.8% MeOH) before Nd elution by the eluent [0.04 M $HNO_3$-99.8% MeOH(1:9)]. The recovery of Nd was more than 94%, regardless of Al contents. Taking the 9 to 13 mL fraction of eluate was effective to purely isolate Nd.

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Identification and characterization of allergens of Chironomus fkavuoynys adults (Chironomidae, Diptera) in mice (노랑털깔따구(Chironomus flaviplumus) 성충의 알레르기 항원단백 분석)

  • 이한일;이상화
    • Parasites, Hosts and Diseases
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    • v.34 no.1
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    • pp.35-48
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    • 1996
  • Non-biting midges fchironomidae, Dipteral are one of the largest insect families, which are distributed worldwidely and are found in nearly all types of inland waters. They are known to be aggressive inhalant allergens which cause allergenic diseases. In this study, the crude antigens of Chironomus SavipLumn adults which are most widely distributed in Korea were extracted. and their allergens were analysed with the sera from experimentally sensitized mice. The mice were immunized with $1{\;}\mu\textrm{g}{\;}or{\;}10{\;}\mu\textrm{g}$ of the crude antigens, respectively, and the specific serum IgE levels were measured by both ELISA and passive cutaneous anaphylaxis (PCA) techniques. The highest levels of both total IgE and chironomid-specific IgE were found in the mouse sera obtained after 9 weeks of the first infection with $1{\;}\mu\textrm{g}$ crude antigen. The crude antigen was separated into 16-18 protein bands on gel by SDS-PAGE. The crude extract was assessed by SDS-PAGE/immunoblot analysis. One IgE-binding band (65 kDa) was detected by developing with colorimetric substrate, and 4 IgE-binding bands (65, 52, 35 and 25 kDa) by developing with CSPD chemiluminescent substrate. The SDS-PAGE gel of the crude extract of chironomid adults was equally cut into 30 pieces and each of them was eluted to isolate proteins by molecular weight, and the allergenicity of each eluate was assessed by applying P-K test on rats. Proteins of 65, 35 and 15 KDa showed the highest P-K titer (${\times}512$) which was 16 times higher than that of the crude extract (${\times32}$). The P-K titer of 52 kDa protein was also 4 times higher ($128{\times}$) than that of the crude extract, whereas the 25 kDa protein poorly responded, which seemed not antigenic. In conclusion, the present result in mice demonstrated that adults of Chironomus fcuiplumus, a predominent species in Korea, cause allergenic diseases and the main allergens are 65, 52, 35 and 15 kDa proteins, of which 65 kDa protein seems to be a main allergen.

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Simultaneous Determination of Titanium, Zirconium and Niobium by Reactor Neutron Activation (원자로 중성자에 의한 티탄, 지르코늄 및 니오브의 동시 정량)

  • Chul Lee;Yung Chang Yim;Koo Soon Chung
    • Journal of the Korean Chemical Society
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    • v.18 no.1
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    • pp.40-46
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    • 1974
  • The fission neutron reactions of $^{47}Ti(n.p)^{47}Sc$ and $^{93}Nb(n,{\alpha})^{90m}Y$, along with epicadmium neutron reaction of $^{96}Zr(n,{\gamma})^{97}Zr$ were used for the simultaneous determination of Ti, Nb and Zr in synthetic mixture. Prior to neutron irradiation, Ti, Zr and Nb in the mixture were separated together in one group through the cation exchange column of Dowex $50{\times}8$ resin using 0.5 M ${\alpha}$-hydroxy-iso-butyric acid as the eluent. After irradiation of the eluate the product nuclides, $^{97}Zr$, ^{47}Sc$ and ^{90m}Y$, were eluted sequentially through the same column with 0.5 M ${\alpha}$-HIBA, 0.5 M ${\alpha}$-HIBA-1 N HNO_3 and 0.5 M ${\alpha}$-HIBA-2 N HNO_3$ solution, respectively. The gamma-ray spectrometry was used for the measurement of the gamma-ray activities of the eluted nuclides. The detection limits of Nb, Ti and Zr were found to be 0.2 %, 0.01 % and 0.002 %, respectively.

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Study on Synthesis of 68GeO2 and Behavior of 68Ga3+ for Generator Column (Generator 컬럼용 68GeO2 합성 및 68Ga3+의 거동에 관한 연구)

  • Kim, Gun Gyun;Lee, Jun Young;Kim, Sang Wook;Hur, Min Gu;Yang, Seung Dae;Park, Jeong Hoon
    • Journal of Radiation Industry
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    • v.10 no.4
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    • pp.189-192
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    • 2016
  • $^{68}Ga$ has emerged as a promising candidate for non-invasive diagnostic imaging within Positron Emission Tomography (PET) because of its advantageous radiochemical characteristics ($t_{1/2}=68min$, ${\beta}^+$ yield ~89%). $^{68}Ga$ forms a stable chelation with various ligands and it is possible to be quickly and easily study using a $^{68}Ge/^{68}Ga$ generator. Commercial $^{68}Ge/^{68}Ga$ generators are chromatographic system using the inorganic materials such as alumina and tin dioxide which are employed as column matrixes for $^{68}Ge$. In this study, we tried out to make $^{68}Ge/^{68}Ga$ generator system with the $^{68}GeO_2$ microstructures for column matrix. $^{68}Ge$ tends to have stable bond with oxide as $^{68}GeO_2$ microstructures. The $^{68}GeO_2$ has been synthesized by hydrolysis of $GeCl_4$ (sol-gel method) and characterized by X-ray diffraction and scanning electron microscope for geometrical analysis. The stability of $GeO_2$ was tested using eluents with diverse solvents(water, ethanol and 0.1 N HCl). The radioactivity of $^{68}Ga^{3+}$ in eluate through $GeO_2$ was measured to prove a function as column material for a generator.

Validation of an analytical method of dieckol for standardization of Ecklonia cava extract as a functional ingredient (감태추출물의 기능성원료 표준화를 위한 지표성분 dieckol의 분석법 검증)

  • Xu, Yan;Kim, Eun Suh;Lee, Ji-Soo;Kim, Gun-Hee;Lee, Hyeon Gyu
    • Korean Journal of Food Science and Technology
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    • v.51 no.5
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    • pp.420-424
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    • 2019
  • An HPLC analysis method was developed and standardized for the detection of dieckol as a functional food ingredient in Ecklonia cava extracts. HPLC was performed using a Capcell Pak C18 column ($250{\times}4.6mm$, $5{\mu}m$) with a gradient elution of water and acetonitrile, both containing 0.1% (v/v) trifluoroacetic acid, at a flow rate of 1.0 mL/min at $25^{\circ}C$. The eluate was detected at 230 nm. For validation, the specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of dieckol were measured. The calibration curve for the detection of dieckol had high linearity ($R^2=0.9994$), with LOD and LOQ values of 0.38 and $1.16{\mu}g/mL$, respectively. Recovery of the quantified compound ranged from 99.61 to 100.71%. The relative standard deviation values of the intra-day and inter-day precisions were less than 1.7 and 1.25%, respectively. These results indicate that the reported HPLC method is simple, reliable, and reproducible for the detection of dieckol in Ecklonia cava extracts.

Animal Skin Irritation and Skin Sensitization Tests of High Intensity Focused Ultrasound System Cartridges (집속형초음파자극시스템 카트리지의 동물실험을 통한 피부자극시험 및 피부 감작성시험)

  • Jun-tae, Kim;Ju-hee, Kim;Kyu-tai, Joo;Kyung-ah, Kim;Ahnryul, Choi;Jae-hyun, Jo;Jin-houng, Jeong
    • The Journal of Korea Institute of Information, Electronics, and Communication Technology
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    • v.15 no.6
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    • pp.477-484
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    • 2022
  • In this study, the cartridge part of the focused ultrasound stimulation system was used as a sample to conduct a skin irritation test and a skin sensitization test through animal experiments among the tests related to GLP (Good Laboratory Practice), a medical device safety evaluation standard. The test was conducted after IACUC approval using 6 female New Zeland White Rabbits. The polar and non-polar stimulation indices were all '0.0'. In addition, in the case of skin sensitization evaluation, 30 guinea pigs approved by IACUC were divided into control and experimental groups, and all induction and induction steps were applied using the eluate itself without separate dilution of the test sample and blank test solution. As a result of the experiment, the skin reaction grade of the control animal was 0 grade, and there was no animal showing more than 1 grade in the skin reaction of the test animal. As a result of both tests, no abnormal skin symptoms were observed, and when applied to the human body to treat patients, the test materials used in the tests will investigate the stability of whether any diseases that cause skin abnormal symptoms will occur.

Radiopharmceutical Factors in the Prepartion of $^{99m}Tc-HMPAO$ Images of the Brain (뇌스캔용 $^{99m}Tc-HM-PAO$의 방사성 동위원소표지에 영향을 미치는 인자에 대한 연구)

  • Yeom, Mi-Kyoung;Kim, Sang-Eun;Lee, Dong-Soo;Chung, June-Key;Lee, Myung-Chul;Koh, Chang-Soon
    • The Korean Journal of Nuclear Medicine
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    • v.25 no.1
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    • pp.117-121
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    • 1991
  • Technetium-99m-hexamethylpropyleneamine oxime $(^{99m}Tc-HM-PAO)$ is a neutral-lipophilic chelate which is used for scanning cerebral blood flow. The labeling efficiencies of $^{99m}Tc-HM-PAO$ is known to be sensitive to the amount of pertechnetate added and the quality of the pertechnetate. Because of these factors, the manufacture recommends that HM-PAO kits be reconstituted with a maximum of 30 mCi pertechnetate which was eluted <4 hr earlier from a generator which had been eluted < 24 hr previously. So we measured the labelling efficiencies and the decomposition rate constant according to the amount of pertechnetate added, the volume of pertechnette added, and generator in-growth time. We used the 3-system chromatographic methods (paper & ITLC-SG chromatography) which analyzed the labelling efficiencies of the $^{99m}Tc-HM-PAO$. There was no significant difference in labelling efficiencies between variable pertechnetate acitvities added. ($39.9{\pm}4.9\;mCi:\;87.8{\pm}5.1\;(%)$, $60.8{\pm}5.0\;mCi:\;90.7{\pm}2.2\;(%)$, $79.0{\pm}6.0\;mCi:\;86.8{\pm}3.9\;(%)$, $106.6{\pm}11.6\;mCi:\;87.7{\pm}1.2\;(%)$, p>0.05) No significant difference in labelling efficiencies were found between pertechnetate of 4ml and 5ml. (4ml : $89.1{\pm}3.2(%)$, 5ml: $87.3{\pm}4.0(%)$, p>0.05). There was no difference between 1-6 and 10-48 hr of generator in-growth time. (1-6 hr: $87.8{\pm}4.0(%)$, 10-48 hr: $89.6{\pm}1.6(%)$, p>0.05) The mean value of decomposition rate constant was $0.196{\pm}0.097\;(hr^{-1})$, and there were no difference according to the amount of pertecnetate added and the volume of pertecnetate added, ($39.9{\pm}4.9\;mCi:\;0.208{\pm}0.059\;(hr^{-1})$, $60.8{\pm}5.0\;mCi:\;0.191{\pm}0.100\;(hr^{-1})$ $79.0{\pm}6.0\;mCi:\;0.192{\pm}0.118\;(hr^{-1})$, $106.6{\pm}11.6\;mCi:\;0.212{\pm}0.030\;(hr^{-1})$, p>0.05, 4 ml: $0.200{\pm}0.074\;(hr^{-1})$, Sml: $0.193{\pm}0.115\;(hr^{-1})$, p>0.05). In the case of using the first eluate, the labelling efficiency of $^{99m}Tc-HM-PAO$ W3S 82.1%. These data suggest that there were no significant alteration in labelling efficiency of $^{99m}Tc-HM-PAO$ according to the considerable range of pertechnetate activities and volume added, and generator in-growth time. Also, it was shown that one vial of HM-PAO kit supplied the $^{99m}Tc-HM-PAO$ which was used for 3-4 patients.

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