• Title/Summary/Keyword: Column extraction

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Stabilization of Arsenic in Soil around the Abandoned Coal-Mine Using Mine Sludge Pellets (광산슬러지 펠렛을 이용한 폐석탄광 주변 토양 내 비소 안정화 연구)

  • Ko, Myoung-Soo;Ji, Won-Hyun;Kim, Young-Gwang;Park, Hyun-Sung
    • Economic and Environmental Geology
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    • v.52 no.1
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    • pp.29-35
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    • 2019
  • The purpose of this study was to assess the applicability of acid mine drainage sludge (AMDS) pellets for the arsenic (As) stabilization and to suggest an evaluation method for arsenic stabilization efficiency in soil around abandoned coal mines. The soil samples were collected from the agricultural field around Ham-Tae, Dong-Won, Dong-Hae, and Ok-Dong coal mine. The As concentration in soil was exceeding the criteria of soil pollution level, except for Ham-Tae coal mine. The AMDS pellets are more appropriate to use by reducing dust occurrence during the transport and application process than AMDS powder. In addition, AMDS pellets were maintained the As stabilization efficiency. The application of AMDS pellets for the As stabilization in soil was assessed by column experiments. The AMDS pellets were more effective than limestone and steel slag, which used as the conventional additives for the stabilization process. The As extraction by $0.43M\;HNO_3$ or $1M\;NaH_2PO_4$ solution were appropriate evaluation methods for evaluation of As stabilization efficiency in the soil.

Determination of Sodium Alginate in Processed Food Products Distributed in Korea

  • Yang, Hyo-Jin;Seo, Eunbin;Yun, Choong-In;Kim, Young-Jun
    • Journal of Food Hygiene and Safety
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    • v.36 no.6
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    • pp.474-480
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    • 2021
  • Sodium alginate is the sodium salt of alginic acid, commonly used as a food additive for stabilizing, thickening, and emulsifying properties. A relatively simple and universal analysis method is used to study sodium alginate due to the complex pretreatment process and extended analysis time required during the quantitative method. As for the equipment, HPLC-UVD and Unison US-Phenyl column were used for analysis. For the pretreatment condition, a shaking apparatus was used for extraction at 150 rpm for 180 minutes at room temperature. The calibration curve made from the standard sodium alginate solution in 5 concentration ranges showed that the linearity (R2) is 0.9999 on average. LOD and LOQ showed 3.96 mg/kg and 12.0 mg/kg, respectively. Furthermore, the average intraday and inter-day accuracy (%) and precision (RSD%) were 98.47-103.74% and 1.69-3.08% for seaweed jelly noodle samples and 99.95-105.76% and 0.59-3.63% for sherbet samples, respectively. The relative uncertainty value was appropriate for the CODEX standard with 1.5-7.9%. To evaluate the applicability of the method developed in this study, the sodium alginate concentrations of 103 products were quantified. The result showed that the detection rate is highest from starch vermicelli and instant fried noodles to sugar processed products.

Analysis of coenzyme Q10 in human plasma by high performance liquid chromatography (고성능액체크로마토그라피를 이용한 혈장 내 코엔자임 큐텐 분석)

  • Park, Yong-Sun;Park, Sang-Boem;Song, Sean-Mi;Kim, Yong-Woo;Lee, Kyoung-Ryul
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.514-518
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    • 2009
  • Coenzyme $Q_{10}$($CoQ_{10}$), a vitamin E-like substance, represents a components of the complex antioxidant system of the human organism. $CoQ_{10}$ levels in human plasma were determined by high performance liquid chromatography (HPLC) with UV detection. It was dissociated from lipoproteins by methanol and extracted into n-hexane with liquid-liquid extraction procedure, after centrifugation, the supernatant was dried under nitrogen gas stream. The residue was dissolved in the absolute ethanol. Determination of $CoQ_{10}$ was performed on a $C_{18}$ reversed-phase analytical column with ultraviolet detection at 275 nm and the mobile phase containing 15% (v/v) ethanol in methanol at a flow rate of 1.7 mL/min. The low limit of quantitation was 0.02 mg/L (S/N=10), the linearity between the concentration and peak height is from 0.1 to 2.0 mg/L. Twenty-four randomly selected plasma samples from apparently healthy, 27 to 44 year old individuals (males and females) were analyzed for total $CoQ_{10}$. The average level in these subjects was $0.62{\pm}0.13mg/L$ with the range of 0.41-0.98 mg/L. This method has a specific and a sufficient limit of quantitation (LOQ) for analysis of $CoQ_{10}$ in human plasma in both a clinical study and research at laboratories.

Elucidation of new anti-impotency analogue in food (식품 중 발기부전치료제 유사물질 규명)

  • Suh, Junghyuck;Choi, Jangduck;Park, Kunsang;Hu, Soojung;Yoon, Taehyung;Kim, Eunju;Han, Seungwoo;Kim, Sohee;Lee, Kwangho;Kwan, Sungwon;Kim, Deukjoon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.345-353
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    • 2009
  • The new anti-impotency analogue was identified in food source. Detection of this analogue was accomplished through screening of food samples by liquid chromatography/photodiode array detector. The spectrum pattern of analogue compound was similar to that observed for hongdenafil which was analogue of sildenafil. This new compound was isolated and purified using the liquid-liquid extraction, thin layer chromatography, column chromatography and preparative HPLC. And then those structure were identified using analytical instruments such as HPLC/PDA, LC/MS/MS and NMR. The compound was given a name to oxohongdenafil which was replaced with acetyl oxoethylpiperazinyl residue instead of sulfonyl piperazine group of sildenafil. The regulation for the abovementioned analogue, oxohongdenafil, was established by Standard of Korean food code.

Sensitive determination of paroxetine in canine plasma by liquid chromatography-tandem mass spectrometry (LC-MS/MS) (LC-MS/MS를 이용한 비글견 혈장 중 파록세틴의 고감도 분석)

  • Chang, Kyu Young;Kang, Seung Woo;Han, Sang Beom;Youm, Jeong-Rok;Lee, Kyung Ryul;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.138-146
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    • 2007
  • A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

Determination of volatile and residual iodine during the dissolution of spent nuclear fuel (사용 후 핵연료 용해 중 휘발 및 잔류 요오드 분석)

  • Kim, Jung Suk;Park, Soon Dal;Jeon, Young Shin;Ha, Young Keong;Song, Kyuseok
    • 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.

Analysis of clenbuterol in bovine muscle and milk by LC-ESI/MS/MS (LC-ESI/MS/MS를 이용한 소고기와 우유에서의 클렌부테롤 분석)

  • Hong, Selyung;Jeong, Jiyoon;Park, Hyejin;Lee, Soonho;Lee, Jongok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.535-542
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    • 2008
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

Antioxidant activity of partially purified extracts isolated from Acanthopanax sessiliflorum Seeman (오가피 분획 추출물의 항산화효과)

  • Im, Kyung-Ran;Kim, Mi-Jin;Jung, Teak-Kyu;Yoon, Kyung-Sup
    • KSBB Journal
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    • v.23 no.4
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    • pp.329-334
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    • 2008
  • The antioxidant activity and the qualitative analysis of Acanthopanax sessiliflorum Seeman were studied by partially purified extract using various methods: extraction by using ethanol solutions and temperatures, and absorption to Diaion HP20 column chromatography using 10%, 20%, 40%, 60% ethanol solutions. Major constituents, chlorogenic acid, caffeic acid, eleutheroside E, was determinated by HPLC method in Acanthopanax sessiliflorum S. 10% and 20% ethanol solutions contain chlorogenic acid (3.020$\pm$0.080%, 20.500$\pm$1.150%, respectively). 40% ethanol solution contains caffeic acid and eleutheroside E (12.270$\pm$0.360%, 1.670$\pm$0.140%, respectively). Diaion HP20 fractions (10%, 20%, 40%, 60% ethanol solutions) showed the scavenging activity of radicals and reactive oxygen species with the $IC_{50}$ values of $81.534{\pm}0.992{\mu}g/ml$, $1.748{\pm}0.098{\mu}g/ml$, $11.487{\pm}1.768{\mu}g/ml$, $21.960{\pm}0.547{\mu}g/ml$ against 1,1-diphenyl-2-picrylhydrazly radical and $1713.548{\pm}34.565{\mu}g/ml$, $131.419{\pm}2.235{\mu}g/ml$, $200.681{\pm}2.444{\mu}g/ml$, $757.897{\pm}6.868{\mu}g/ml$ against superoxide radicals in the xanthine/xanthine oxidase system, respectively. Especially, 20% and 40% ethanol fractions showed more antioxidant activity than dl-$\alpha$-tocopherol. These results suggest that Acanthopanax sessiliflorum S. extract and Diaion HP20 fractions may be useful as a potential source of nutraceutical and cosmetic products.

Isolation and Identification of Flavonoids from Corn Silk (옥수수수염에 함유된 Flavonoids의 분리 및 동정)

  • Kim, Sun-Lim;Kim, Mi-Jung;Lee, Yu-Young;Jung, Gun-Ho;Son, Beom-Young;Lee, Jin-Seok;Kwon, Young-Up;Park, Yong-Il
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.59 no.4
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    • pp.435-444
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    • 2014
  • This study was carried out to isolate and characterize the flavonoids present in corn silks. Maysin content in the unpollinated corn silks (Kwangpyeongok) showed its highest level at 3 days after silking, and decreased thereafter, while the content of open pollinated silks were consistently decreased after silking. This result indicates that the maysin content is considerably affected by the pollination of corn silk. Unpollinated corn silks were collected with excising, and ethanol employed to extract flavonoids at common temperature for 9 days. After extraction, chlorophyll, lipids etc. were removed with methylene chloride, then submitted to flash column cartridge ($150{\times}40mm$ i.d.) packed with a preparative $RP-C_{18}$ bulk packing material ($125{\AA}$, $55-105{\mu}m$), and monitored at 352 nm. Four fractions, fraction-I, -II, -III, and -IV, were isolated from ethanolic extract of corn silks. Absorption spectrum of fraction I showed its maximum intensity (${\lambda}_{max}$) at 327 nm and 239 nm, fraction-II showed its maximum intensity at 339 nm and 274 nm, fraction-III showed its maximum intensity at 345 nm and 277 nm, and fraction-IV showed its maximum intensity at 352 nm, 270 nm, 257 nm, respectively. On the baisis of ESI micro-TOF analysis, fraction-I was identified as chlorogenic acid (m/z 355, 3-(3,4-dihydroxycinnamoyl) quinic acid, $C_{16}H_{18}O_9$), fraction-II identified as a mixture of chlorogenic acid and luteolin 3'-methyl ether 7-glucuronosyl-($1{\rightarrow}2$)-glucuronide (m/z 653, $C_{28}H_{28}O_{18}$), fraction-III identified as a mixture of chlorogenic acid luteolin 7-O-neohesperidoside (m/z 595, $C_{27}H_{30}O_{15}$), and luteolin 3'-methyl ether 7-glucuronosyl-($1{\rightarrow}2$)-glucuronide, and fraction-IV identified as maysin (m/z 577, 2"-O-${\alpha}$-L-rhamnosyl-6-C-(6-deoxy-xylohexose-4-ulosyl)luteolin, $C_{27}H_{28}O_{14}$), respectively. From the ethanolic extract of corn silks, fraction-I was obtained about 35 mg/100 g F.W., fraction-II was about 48 mg/100 g F.W., fraction-III was about 46 mg/100 g F.W., and fraction-IV was about 138 mg/100 g F.W., respectively.

Purification and Characterization of Oriental Pear(Niitaka, Pyrus pyrifolia Nak.) Protease (동양배(신고(新高)) Protease의 정제(精製) 및 성질(性質)에 관(關)하여)

  • Kim, Seung Yeol;Chung, Hai Jung;Kim, Seung Kyeom;Shin, Cheol Seung
    • Korean Journal of Agricultural Science
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    • v.16 no.2
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    • pp.225-238
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    • 1989
  • These studies were conducted to investigate the extraction, purification and characterization of oriental pear (Niitaka. Pyrus pyrifolia Nak.) protease, and the results obtained were as follows: 1. Oriental pear protease was effectively extracted by the method of homogenizing pear pulp with 0.7 volume of 0.1M-sodium phosphate buffer, pH 6.5 containing 5mM-cysteine, 40mM-2-mercaptoethanol and 2mM-EDTA at 10,000 rpm for 5 min. 2. The protease was purified by ammonium sulfate fractionation, Sephadex G-100 filtration and DEAE-Sephadex A-50 column chromatography, and the purified enzyme gave a single protein band on polyacrylamide gel electrophoresis. 3. The specific activity of purified enzyme was 29.65 unit/mg protein and the yield was 7.22%. 4. The moecular weight of the protease was estimated to be about 51,000 by SDS-polyacrylamide gel electrophoresis, and the enzyme had Km value of 54.5 mg/ml for casein. 5. The purified enzyme had a maximum activity at pH 6.0 and $50^{\circ}C$, and was stable from pH 5.5-6.5 and at temperatures below $50^{\circ}C$ 6. Casein was a better substrate for this protease compared to hemoglobin. 7. The enzyme activity was markedly inhibited by p-chloromercuribenzoic acid and heavy metal salts such as $HgCl_2$ and $MnSO_4$ also considerably inhibited the enzyme activity.

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