• Title/Summary/Keyword: 용출법

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Determination of new anti-HIV agents, the KR-V series, in rat plasma using microbore high-performance liquid chromatography (HPLC를 이용한 랫드혈장내 새로운 항HIV제 KR-V series의 분석법)

  • Lee, Young-mi;Park, Myung-jin;Kim, Jin-suk;Shin, Ho-chul
    • Korean Journal of Veterinary Research
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    • v.40 no.4
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    • pp.741-746
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    • 2000
  • We have developed a rapid, simple and precise high-performance liquid chromatographic (HPLC) method using an UV detection system for the determination of new anti-HIV candidates, nineteen KR-V compounds, in rat plasma. We used a analytical columnn of $C_{18}$ ($5{\mu}m$, $250{\times}2.0mm$ I.D.) and a mobile phase of water and ACN mixture (40/60, v/v). Under these conditions, all the KR-V compounds were readily separated from plasma with retention times of 4-12 min. The limits of quantitation for the 19 KR-V compounds were 15-30 ng/ml. The recoveries from the plasma were higher than 85% (C.V.<10%) with exception of KR-V 2, 7 and 15. The compounds KR-V 2, 7 and 15, containing ester moieties, were found to be unstable in plasma. This result suggests that esters, like KR -V 2, 7 and 15, should be excluded from future structure design studies of anti-HIV KR-V agents. In conclusion, the current HPLC method is a valuable analytical tool for investigating the pharmacokinetics of the KR-V series in rats.

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Optimization of mixing ratio in preparation of gluten-free rice udon through response surface methodology (반응 표면 분석법을 이용한 글루텐 프리 쌀 우동 제조 최적화)

  • Park, Se-Jin;Eun, Jong-Bang
    • Korean Journal of Food Science and Technology
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    • v.53 no.6
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    • pp.739-748
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    • 2021
  • This study focuses on the use of rice in the production of gluten-free rice udon (GFU) through an optimized mixing ratio, using the Box-Behnken response surface methodology (RSM). Different additional levels of rice flour (A, 40-60 g), acetylated distarch adipate (B, 10-20 g), and trehalose (C, 0-3 g) were used as variables, while water absorption level, volume, cooking loss, solid yield, lightness, texture properties, proximate compositions of GFU and turbidity of cooking water were set as responses in the RSM design model. The optimum mixing ratio for the preparation of gluten-free rice udon was obtained for 60.00 g of rice flour, 18.81 g of acetylated distarch adipate without the addition of trehalose. The response values of the optimized samples were water absorption (60.94%), volume (34.94%), turbidity of the cooking water (0.37), cooking loss (4.77%), solid yield (1.55 g), lightness value (70.04), hardness (2.53 N), springiness (0.18), gumminess (10.45 N), chewiness (1.83 N), and cohesiveness (2.89). This study has shown that rice flour can replace wheat flour to manufacture udon at an optimized mixing ratio successfully derived by statistical estimation method.

New Methods for Separation of Crude Ginseng Saponins (인삼 조사포닌의 새로운 분리 방법)

  • Shin, Ji-Young;Choi, Eon-Ho;Wee, Jae-Joon
    • Korean Journal of Food Science and Technology
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    • v.33 no.2
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    • pp.166-172
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    • 2001
  • In order to increase ginsenoside content, to reduce chemical change, to shorten extracting procedure, new methods of extraction and fractionation of crude ginseng saponin were established and compared for their chemical composition. Those are hot MeOH extraction/n-BuOH fractionation (BuOH method) and hot MeOH extraction/Diaion HP-20 adsorption/MeOH elution (HP-20 method), which are already known methods, and additional three new methods: hot MeOH extraction/cation AG 50W $adsorption/H_2O$ elution/n-BuOH extraction (AG 50W method), cool MeOH extraction/Diaion HP-20 adsorption/MeOH elution (cool extraction method) and direct extraction with EtOAc/n-BuOH (direct extraction method). AG 50W method provided a crude saponin showing the highest content of ginsenosides of 61.5% and the lowest contents of protein and free amino acids of 0.93% and 0.19%, respectively. The protein content was the highest as 14.18% in the crude saponin by HP-20 method, while free sugar content was the highest as 13.5% by BuOH method, indicating that these are factors that lower the rate of ginsenoside in crude saponins by those methods. On the other hand, it was revealed that AG 50W method produced large amount of prosapogenins during the pass through the cation exchange resin (AG 50W) column being strongly acidic. Crude saponin from direct extraction method showed relatively higher composition of ginsenoside $Rg_1$ and Re. The results suggest that contents and composition of ginsenosides and other chemical components in crude ginseng saponin greatly depend on the condition of the extraction and fractionation.

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Stabilization of Heavy Metal Contaminated Paddy Soils near Abandoned Mine with Steel Slag and CaO (제강슬래그와 CaO를 이용한 폐광산 주변 중금속 오염 농경지 토양의 안정화 처리 연구)

  • Son, Jung-Ho;Roh, Hoon;Lee, Sun-Young;Kim, Sung-Kyu;Kim, Gil-Hong;Park, Joong-Kyu;Yang, Jae-Kyu;Chang, Yoon-Young
    • Journal of Soil and Groundwater Environment
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    • v.14 no.6
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    • pp.78-86
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    • 2009
  • Applicability of CaO and steel slag as stabilizers in the treatment of field and paddy soils near Pungjeong mine contaminated with arsenic and cationic heavy metals was investigated from batch and column experiments. Immobilization of heavy metals was evaluated by TCLP dissolution test. Immobility of heavy metal ions was less than 15% when steel slag alone was used. This result suggests that $Fe_2O_3$ and $SiO_2$, known as the major component of steel slag, have little effect for the immobilization of heavy metal ions due to acidity of TCLP solution. Immobilization of cationic heavy metals was little affected by the ratio of CaO and steel slag while arsenic removal was increased as the ratio of steel slag to CaO increased. In the column test, concentrations of both arsenic and cationic heavy metals in effluents were below the water discharge guideline over the entire reaction period. This result can be explained by the immobilization of cationic heavy metals from the increased pH in soil solution as well as by the formation of insoluble $Ca_3(AsO_4)_2$. From this work, it is possible to suggest that arsenic and cationic heavy metals can be concurrently stabilized by application of both CaO and steel slag.

Characterization on the Behavior of Heavy Metals and Arsenic in the Weathered Tailings of Songcheon Mine (송천광산의 풍화광미 내 중금속 및 비소 거동 특성)

  • Lee, Woo-Chun;Kim, Young-Ho;Cho, Hyen-Goo;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.2
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    • pp.125-139
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    • 2010
  • Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

Matrix effect on the Determination of Inorganic Priority Pollutants in Sludges (오니 시료중의 무기 Priority Pollutants의 분석 과정에 미치는 매질의 영향)

  • Lee, Huk-Hee;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.11 no.4
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    • pp.297-304
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    • 1998
  • The three analysis methods, EPA method 3050, the method offered by Ministry of Environment in Korea, and modified method corrected in this laboratory, were studied to investigate the effect of matrix on the analysis of inorganic priority pollutants. 7 inorganic priority pollutants(Ni, Cr, Cu, Zn, Pb, Cd, Hg) were spiked to the plating, leather, paper, electric, and dye sludges. Mean recovery of the elements except Hg was 95.5% when the procedure of EPA method was applied. However, recovery by the two other extraction methods showed 11.1% and 27.7%, respectively. Digestions were done by MDS (microwave digestion system) and $HNO_3+HClO_4$ methods. To study organic and inorganic matrix effect, samples were made by adding triethanol amine as a organic matrix and $FeCl_3{\cdot}6H_2O$+$AlCl_3{\cdot}6H_2O$ as a inorganic matrix, respectively. The extracts were analyzed by AAS and HG-AAS. Mean recovery of the elements by the $HNO_3+HClO_4$ procedure, except Hg, gave better result than that of the MDS method. Mean recovery of elements was decreased when organic and inorganic matrices were added in the sludge samples. The procedure of MDS and $HNO_3+HClO_4$ digestion gave higher recoveries than that of direct analysis. In general, the results of the studies showed a significant matrix effect on the inorganic priority pollutants analysis in sludges.

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Improvement of Analytical Method for Residue Pesticides in Herbal Medicines Using Macroporous Diatomaceous Earth Column (다공성 규조토 컬럼을 이용한 한약재 중 잔류농약 분석법 개선)

  • Hwang, Jeong-In;Jeon, Young-Hwan;Kim, Hyo-Young;Kim, Ji-Hwan;Ahn, Ji-Woon;Seok, Da-Rong;Lee, Yoon-Jeong;Park, Ju-Young;Kim, Do-Hoon;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.15 no.2
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    • pp.140-148
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    • 2011
  • The official analytical method of residue pesticides in herbal medicines by KFDA cannot be applied to all of the pesticides and herbal medicines because of various active materials in herbal medicines and various physicochemical properties of pesticides. Moreover, liquid-liquid partition uses harmful solvents such as methylene chloride and is consuming a lot of time and effort. In order to improve the problems, we have studied for the availability of the analytical method applying the macroporous diatomaceous earth (MDE) column instead of liquid-liquid partition to simultaneously analyze five pesticides in two dried herbal medicines. The results showed that the recovery rates of acetamiprid and azoxystrobin in Astragalus root by GC/ECD ranged from 89.6 to 94.1%, from 86.8 to 94.4%, respectively, and those of bifenthrin, chlorfenapyr, chlorpyrifos in Cnidii Rhizoma by GC/MS ranged from 83.6 to 88.4%, from 77.4 to 83.8%, from 82.6 to 84.3%, respectively. Also, the coefficients of variation (CV) for triplication ranged from 0.5 to 1.7%. The results satisfied the criteria of residue pesticide analysis, setting 70~120% for the recovery rate and below 10% for the coefficient of variation. The improved methods are safer to residue pesticide analysts, faster and less laborious than the KFDA official method.

Influence of Surface Treatment of SiO$_2$ and Stirring Rate on Fragrant Oil Release Behavior of Poly($\varepsilon$-caprolactone) Microcapsules (실리카의 표면 처리와 교반 속도가 폴리카프로락톤 마이크로캡슐의 향유 방출 거동에 미치는 영향)

  • 박수진;양영준;이재락;서동학
    • Polymer(Korea)
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    • v.27 no.5
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    • pp.464-469
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    • 2003
  • In this work, the fragrant oil release behavior of poly($\varepsilon$-caprolactone) (PCL) microcapsules containing SiO$_2$ was investigated. The SiO$_2$ was chemically treated in 10, 20, and 30 wt% hydrochloric acid and sodium hydroxide. The acid and base values were determined by Boehm's titration technique and $N_2$/77 K adsorption isotherm characteristics, the specific surface area and total pore volume were studied by BET. The PCL microcapsules containing SiO$_2$ and fragrant oil were prepared by oil-in-water (o/w) emulsion solvent evaporation method. The shape and surface of PCL microcapsules were observed using image analyzer and scanning electron microscope (SEM). The fragrant oil release behavior of PCL microcapsules was characterized using UV/vis. spectra. The average diameters of PCL microcapsules were decreased from 35 to 21 $\mu$m with increasing stirring rate. It was found that in the case of acidic treatment the fragrant oil adsorption capacity and release rate were increased due to the increase of specific surface area and acid value. In the case of basic treatment, the fragrant oil adsorption capacity and release rate were decreased due to the decrease of sp ecific surface area and the increase of acid-base interactions between SiO$_2$-NaOH and fragrant oil with increasing base value of SiO$_2$.

Purification of IgG1 Type Mouse Monoclonal Antibodies with DEAE-Trisacryl Chromatography (DEAE-Trisacryl 크로마토그래피법에 의한 IgG1 Type 쥐 단일클론 항체의 분리정제)

  • 최태부;정용근
    • Microbiology and Biotechnology Letters
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    • v.16 no.5
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    • pp.335-342
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    • 1988
  • An anion exchange chromatography was employed for the purification of mouse monoclonal antibodies from ascitic fluid and in vitro cultivation media. After cultivation of hybridomas, Alps 25-3, HCGK, A4W, and KW, producing IgG1, the culture supernatants were harvested by centrifugation, precipitated with 50-60% ammonium sulfate, and dialyzed against 0.025 M Tris-HCI buffer (pH 8.2). Then the dialyzed samples were loaded into a DEAE-Trisacryl M anion exchange column. Monoclonal antibodies bound to the DEAE-Trisacryl M were eluted with 0.025 M Tris-HCI buffer (pH 8.2) containing 30-40 mM NaCl. In ammonium sulfate precipitation, the recovery of the monoclonal antibody was shown to be 90% and 84% from in vitro culture media containing 10% and 2% fetal bovine serum, respectively. On the other hand, the pretreatment by ultrafiltration enhanced the yield up to 91% whereas the purity was lower than that by ammonium sulfate treatment. Subsequently, in the DEAE-Trisacryl M chromatographic separation, the purities and recoveries of all the monoclonal antibodies from both the in vitro culture supernatants and ascitic fluids were 70-80% and 65% respectively. The monoclonal antibody, Alps 25-3 could be further purified with a purity of 95% through an immunoadsorbent chromatography.

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Recycling of the Waste Rock and Tailings from Yangyang Iron Mine (양양철광산 선광 부산물의 순환자원화)

  • Jung, Moon Young;An, Yong Hyeon;Kim, Young Hun
    • Resources Recycling
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    • v.25 no.4
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    • pp.23-31
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    • 2016
  • It was found that there was no problem in recycling by-products (waste rock and tailings) from Yangyang iron mine themselves through matter conversion because they are not hazardous according to results of KSLT method. In case of using tailings as sub-materials of cement, it recommended the use of less than 3% tailings dosage not to exceed 0.6% of total alkali ($R_2O$) content based on standard quality of portland cement (KS L 5201). Non sintered eco-brick corresponding to class 1 quality of recycled clay brick (KS I 3013) can replace 15% of cement with tailings and 100% of general fine aggregate with waste rock from iron mine. As mentioned above, recycling the by-products (waste rock and tailings) as sub-materials of cement and non sintered eco-brick could gain both environmental and economic benefits, that is, reduction of scale and maintenance cost of tailing ponds, decrease of energy use and $CO_2$ emission.