• Title/Summary/Keyword: Column extraction

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Studies on the Development of Natural Preservatives from Natural Products (전통식품 및 천연물에서 천연보존료 개발에 관한 연구)

  • Kim, Hee-Yun;Lee, Young-Ja;Hong, Ki-Hyoung;Kwon, Yong-Kwan;Lee, Ju-Yeun;Kim, So-Hee;Ha, Sang-Chunl;Cho, Hong-Yon;Chang, Ih-Seop;Lee, Chul-Won;Kim, Kil-Saeng
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1667-1678
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    • 1999
  • Certain parts of 190 kinds of medicinal herbs and 171 kinds of original materials of food were extracted by methanol. The extracts were tested their microbial inhibition activities against several food spoilage microorganisms, Micrococcus luteus, Bacillus subtilis, Bacillus cereus, Listeria monocytogenes, Pseudomonas aeruginosa, Salmonella typhimurium, Escherichia coli, Saccharomyces cerevisiae, Candida albicans, Penicillium citrinum, Aspergillus flavus and Aspergillus niger. The methanol extracts of Cornus officinalis, Evodia officinalis, Glycyrrhiza glabra, Salvia miltiorrhiza. Schizandrae fructus, Coptidis rhizoma, aroma hop and bitter hop were shown inhibitory effect on certain species of gram(+) bacteria. Aroma hop and bitter hop were shown inhibitory effect on certain species of gram(-) bacteria. The methanol extract of Salvia miltiorrhiza exhibited a strong antibacterial activities. It was purified by solvent fractionation, silicagel column chromatography, prep. TLC, prep. HPLC. The purified active substance was identified as cryptotanshinone by EIMS, $1^H-NMR,\;{13}^C-NMR$ and DEPT. Cryptotanshinone showed a strong antibacterial activity against gram positive bacteria $(MIC\;:\;3.91{\sim}62.50\;{\mu}g/mL)$. Especially, this compound was the most strong activity against Bacillus subtilis $(MIC\;:\;3.91\;{\mu}g/mL)$.

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Phosphorus Phases in the Surface Sediment of the South Sea (남해 표층 퇴적물에서의 인의 존재상)

  • SON Jaekyung;LEE Tongsup;YANG Han Soeb
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.32 no.5
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    • pp.680-687
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    • 1999
  • To understand the role of shelf sediment in phosphorus biogeochemical cycle, we carried out sequential sediment extraction (SEDEX) of P and porewater analysis on 14 core samples collected in the South Sea of Korea, SEDEX classified P-pools into 5 phases and results are grouped into two categories: reactive P (loosely sorbed-P and Fe bound-P) and refractory P (detrital inorganic-p, authigenic mineral-P and organic-P). Total P concentrations are decreased with sediment depth in all samples as a result of dissolution to porewater. Reactive P comprises about $20\~50\%$ of total P, and iron bound-P is the major form consisting $70\~80\%$ of reactive P-pool. Iron bound-P decreases sharply with depth. Depth profiles of dissolved P concentration in porewater show mirror image of iron bound-P, revealing the role of FeOOH as a regulator of reactive P supply to overlying water column. Authigenic mineral-P consists less than $5\%$ of total P, thus removal of reactive P by converting into refractory P seems inefficient in shelf sediment. This implies that continental shelf sediment sequesters P temporarily rather than permanently. Results show local variation. Nakdong estuary receiving large amount of terrigenous input shows the highest concentration of total P and reactive P. Here iron oxyhydroxides at the surface sediment control the water column flux of P from sediment. Although total P content at the surface is comparable (500$\~$600 ${\mu}g{\cdot}g^{-1}$) between the South Sea and East China Sea, the former contains more iron bound-P and less derital inorganic-P than the latter. Reasons for the difference seem due in part to particle texture, and to biological productivity which depends roughly on the distance from land.

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Method Development for Determination of Chlorogenic Acid and Arbutin Contents in Fruits by UHPLC-MS/MS (UHPLC-MS/MS를 이용한 과일류 중 클로로젠산 및 알부틴 동시분석법 개발)

  • Choi, Young-Ju;Jeon, Jong-Sup;Kim, Woon-Ho;Jung, You-Jung;Ryu, Ji-Eun;Choi, Jong-Chul;Chae, Kyung-Suk;Lee, Jin-Hee;Do, Young-Sook;Park, Young-Bae;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.34 no.5
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    • pp.413-420
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    • 2019
  • In this study, a sample preparation method and a simultaneous determination method by ultra-high performance liquid chromatography coupled with tandem mass spectrometry for 9 isomers of chlorogenic acid and arbutin in fruits were developed. The samples were extracted using 90% methanol (pH 3.0), with the solutions being shaken and then sonicated for 10 min each. After centrifugation at 4,000 rpm for 10 min, the extraction was concentrated under a vacuum at $40^{\circ}C$ using a vacuum evaporator. The residue was dissolved in 5 mL of 5% methanol and filtered through a $0.45{\mu}m$ membrane before UHPLC-MS/MS analysis. The separations were performed on a C18 column with gradient elution of water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid). The specificity, linearity, limit of detection, limit of quantification, accuracy, and precision of the proposed methods were also evaluated.

Metabolites profiling and hypolipidemic/hypocholesterolemic effects of persimmon (Diosyros kaki Thumb.) by different processing procedures: in vitro and in vivo studies (제조방법에 따른 떫은감 (Diosyros kaki Thumb.)의 대사체 프로파일링과 중성지질/콜레스테롤 대사 관련 유전자발현 연구 : in vitro 및 in vivo 연구)

  • Park, Soo-Yeon;Oh, Eun-Kyung;Lim, Yeni;Shin, Ji-Yoon;Jung, Hee-Ah;Park, Song-Yi;Lee, Jin Hee;Choe, Jeong-Sook;Kwon, Oran
    • Journal of Nutrition and Health
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    • v.51 no.4
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    • pp.275-286
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    • 2018
  • Purpose: Our previous study demonstrated that persimmon (Diospyros kaki Thumb.) at different stages of ripening provided different protective effects against high-fat/cholesterol diet (HFD)-induced dyslipidemia in rats. In this study, we compared the metabolites profile and gene expressions related to triglyceride (TG)/cholesterol metabolism in vitro and in vivo after treating with persimmon water extracts (PWE) or tannin-enriched persimmon concentrate (TEP). Methods: Primary and secondary metabolites in test materials were determined by GC-TOF/MS, UHPLC-LTQ-ESI-IT-MS/MS, and UPLC-Q-TOF-MS. The expression of genes related to TG and cholesterol metabolism were determined by RT-PCR both in HepG2 cells stimulated by oleic acid/palmitic acid and in liver tissues obtained from Wistar rats fed with HFD and PWE at 0, 150, 300, and 600 mg/d (experiment I) or TEP at 0, 7, 14, and 28 mg/d (experiment II) by oral gavage for 9 weeks. Results: PLS-DA analysis and heatmap analysis demonstrated significantly differential profiling of metabolites of PWE and TEP according to processing of persimmon powder. In vitro, TEP showed similar hypolipidemic effects as PWE, but significantly enhanced hypocholesterolemic effects compared to PWE in sterol regulatory element-binding protein 2 (SREBP2), HMG-CoA reductase (HMGCR), proprotein convertase subtilisin/kexin type 9 (PCSK9), cholesterol $7{\alpha}-hydroxylase$ (CYP7A1), and low density lipoprotein receptor (LDLR) gene expression. Consistently, TEP and PWE showed similar hypolipidemic capacity in vivo, but significantly enhanced hypocholesterolemic capacity in terms of SREBP2, HMGCR, and bile salt export pump (BSEP) gene expression. Conclusion: These results suggest that column extraction after hot water extraction may be a good strategy to enhance tannins and long-chain fatty acid amides, which might cause stimulation of hypocholesterolemic actions through downregulation of cholesterol biosynthesis gene expression and upregulation of LDL receptor gene expression.

Dealumination of $NH_4Y$-Zeolite to Convert to the Hydrophobic Zeolite by High-Temperature Steam Treatment (소수성 제올라이트로의 변환을 위한 고온 수증기처리에 의한 $NH_4Y$-제올라이트의 탈알루미늄)

  • Kim, Jin-Young;Jeon, Dong-Hwan;Chung, Byung-Hwan;Mo, Se-Young
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.4
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    • pp.420-430
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    • 2005
  • This study was performed to change the hydrophilic $NH_4Y$-zeolite to the hydrophobic one for removal of VOCs by removing the $Al^{3+}$ in the zeolite-structure to increase the Si/Al ratio, for which the three pelleted $NH_4Y$-zeolite samples were contacted separately with the steam of $400^{\circ}C$, $500^{\circ}C$ and $600^{\circ}C$, respectively, in a stainless steel column for 4 hours. Then extraction of the ex-structure aluminum of the hydrolyzed zeolites with the nitric acids of 0.25, 0.50, 0.75, and 0.10 M at $90^{\circ}C$ in 500 mL-flasks, respectively, according to steam temperature were followed. XRD analysises of the dealuminated zeolites showed that the peaks of the zeolites that had been hydrolyzed with the steams of both $500^{\circ}C$ and $600^{\circ}C$ are distorted more with the increase of the concentration of nitric acid used for extraction of the ex-structure aluminums, however, those hydrolyzed with steam of $400^{\circ}C$ became amorphous phase when treated with the all nitric acids of four concentrations. Also the EDX analysises showed that the BET surface areas and TPVS of the zeolites that had been hydrolyzed with the steam of $600^{\circ}C$ were increased with the concentration of the nitric acid when the nitric acids of 0.25 M and 0.5 M had been used but decreased when the nitric acids of 0.75 M and 1.0 M had been used. These results led to the conclusion that both the $600^{\circ}C$ and $500^{\circ}C$-steam and the 0.5 M-nitric acid are appropriate to change the hydrophilic $NH_4Y$-zeolites to the hydrophobic one, which were proven by the measurement of the benzene and tolune-adsorbing capacities showing the same trend as the BET surface area and TPV The Si/Al ratios and water-adsorbing capacities of the dealuminated zeolites were increased and decreased, respectively, with the concentration of the nitric acids so that it showed that the hydrophobicity is increased.

Studies on Development of Protein Food Resources -(Separation of Protein from Korean Cottonseed and its Application to Food)- (단백질(蛋白質) 식량자원(食糧資源)의 개발(開發)에 관(關)한 연구(硏究) -(한국산(韓國産) 면실(綿實)에서 단백질(蛋白質)의 분리(分離) 및 식품(食品)에의 응용(應用))-)

  • Kim, Jun-Pyong;Kim, Chang-Johng;Nam, Chung-Hee
    • Korean Journal of Food Science and Technology
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    • v.9 no.3
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    • pp.211-219
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    • 1977
  • Dehulled and defatted Korean cottonseed flour was extracted with alkaline solution for 30 minutes and had precipitated the crude portein by adjusting pH $1{\sim}12$. The general composition and the amino acid composition of cottonseed protein were analyzed. Crude protein was purified with sephadex G-100 and G-200, and its component had been identified by disc electrophoresis. Toxic gossypol was removed by n-hexane, acetone and other solvents. The results were as follows. (1) pH 5, pH 7 and pH 4 were the best condition of precipitation of curde protein at single, two step and water extraction, respectively. (2) The cottonseed flour which was dehulled and defatted, contained 61.3% of crude protein. (3) The protein which was isolated from cottonseed flour, contained 20% of glutamic acid, and comparatively high levels of essential amino acids. (4) Dehulled cottonseed flour contained 0.97% of total gossypol and could be romoved 70% of total gossypol by extraction with n-hexane. (5) 10-13 bands of water soluble protein were found in disc electrophoresis, and 10-12 bands in protein were isolated by single and two step procedures. (6) The cottonseed protein could be purified by sephadex G-100 and G-200. (7) 10-20% of gossypol-free cottonseed fluor could be used for animal and human comsumption.

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Inhibitory Effects of Ethanolic Extracts from Aster glehni on Xanthine Oxidase and Content Determination of Bioactive Components Using HPLC-UV (섬쑥부쟁이 에탄올 추출물의 잔틴산화효소 저해 효능 및 HPLC-UV를 이용한 유효성분의 함량 분석)

  • Kang, Dong Hyeon;Han, Eun Hye;Jin, Changbae;Kim, Hyoung Ja
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1610-1616
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    • 2016
  • This study aimed to establish an optimal extraction process and high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method for determination of 3,5-dicaffeoylquinic acid (3,5-DCQA) as a part of materials standardization for the development of a xanthine oxidase inhibitor as a health functional food. The quantitative determination method of 3,5-DCQA as a marker compound was optimized by HPLC analysis using a Luna RP-18 column, and the correlation coefficient for the calibration curve showed good linearity of more than 0.9999 using a gradient eluent of water (1% acetic acid) and methanol as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 320 nm. The HPLC-UV method was applied successfully to quantification of the marker compound (3,5-DCQA) in Aster glehni extracts after validation of the method with linearity, accuracy, and precision. Ethanolic extracts of A. glehni (AGEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 30, 50, 70, and 80% ethanol for 3, 4, 5, and 6 h, respectively. Among AGEs, 70% AGE at $70^{\circ}C$ showed the highest content of 3,5-DCQA of $52.59{\pm}3.45mg/100g$ A. glehni. Furthermore, AGEs were analyzed for their inhibitory activities on uric acid production by the xanthine/xanthine oxidase system. The 70% AGE at $70^{\circ}C$ showed the most potent inhibitory activity with $IC_{50}$ values of $77.01{\pm}3.13{\sim}89.96{\pm}3.08{\mu}g/mL$. The results suggest that standardization of 3,5-DCQA in AGEs using HPLC-UV analysis would be an acceptable method for the development of health functional foods.

Remediation of Arsenic Contaminated soils Using a Hybrid Technology Integrating Bioleaching and Electrokinetics (생용출과 전기동력학을 연계한 통합기술을 이용한 비소 오염 토양의 정화)

  • Lee, Keun-Young;Kimg, Kyoung-Woong;Kim, Soon-Oh
    • Journal of Soil and Groundwater Environment
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    • v.14 no.2
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    • pp.33-44
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    • 2009
  • The objective of the study was to develop a hybrid technology integrating biological and physicochemical technologies to efficiently remediate arsenic contaminated lands such as abandoned mine area. The tailing soil samples contaminated with As at a high level were obtained from Songchon abandoned mine, and the content of arsenic and heavy metals as well as physicochemical properties and mineral composition were investigated. In addition, two sets of sequential extraction methods were applied to analyze chemical speciations of arsenic and heavy metals to expect their leachability and mobility in geoenvironment. Based on these geochemical data of arsenic and heavy metal contaminants, column-type experiments on the bioleaching of arsenic were undertaken. Subsequently, experiments on the hybrid process incorporating bioleaching and electrokinetics were accomplished and its removal efficiency of arsenic was compared with that of the individual electrokinetic process. With the results, finally, the feasibilty of the hybrid technnology was evaluated. The arsenic removal efficiencies of the individual electrokinetic process (44 days) and the hybrid process incorporating bioleaching (28 days) and electrokinetics (16 dyas) were measured 57.8% and 64.5%, respectively, when both two processes were operated in an identical condition. On the contrary, the arsenic removal efficiency during the bioleaching process (28 days) appeared relatively lower (11.8%), and the result indicates that the bioleaching process enhanced the efficacy of the electrokinetic process as a result of mobilization of arsenic rather than removed arsenic by itself. In particular, the arsenic removal rate of the electrokinetics integrated with bioleaching was observed over than 2 times larger than that obtained by the electrokinetics alone. From the results of the study, if the bioleaching which is considered a relatively economic process is applied sufficiently prior to electrokinetics, the removal efficiency and rate of arsenic can be significantly improved. Consequently, the study proves the feasibility of the hybrid process integrating both technologies.

Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발)

  • Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.201-210
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    • 2017
  • BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

A study of relationship between stomach cancer and selenoproteins in Korean human blood serum (한국인 혈청에서의 셀레노 단백질과 위암과의 상관관계 연구)

  • Park, Myungsun;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.417-424
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    • 2015
  • In this study, the relationship between selenoprotein concentrations in blood and stomach cancer have been searched for Korean. The concentration of each selenoprotein in blood serum was analyzed and the correlation between the concentration and stomach cancer was studied to find a potential for using Selenium as a biomarker. In concentration determination, a simple calibration curve method was used with the monitoring of m/z 78 without the use of solid phase extraction. This is a lot more simple than the method using SPE with post column isotope dilution. The result obtained from the analysis of CRM BCR-637, 72.20±3.35 ng·g−1, showed similar value of reference value (81±7 ng·g−1). The total concentration of Se for the controlled group, cardiovascular patients group, was 105.70±21.20 ng·g−1. This value was the same as normal healthy person reported earlier. Each selenoprotein concentration of GPx, SelP and SeAlb was 26.12±7.84, 65.15±14.50, 14.43±6.99 ng·g−1, respectively. The distribution of each selenoprotein was 24.7%, 61.6%, and 13.7%, which was similar to the normal person. The result of stomach cancer patients, the total concentration of Se was 76.11±28.12 ng·g−1 and each concentration of GPx, SelP and SeAlb was 15.41±9.01, 50.83±17.91, and 9.87±5.21 ng·g−1, respectively. The total and each selenoprotein concentration level showed significant decrease for the stomach cancer patients. The level of decrease was 41.0% for GPx, 22.0% for SelP, and 31.6% for SeAlb. However, the distribution of each selenoprotein was not much different. Either total Selenium or each selenoprotein could be used as a possible index for the diagnosis of cancer. However, in age group study, it is shown that young age group (30's-40's) did not show much difference.