• Title/Summary/Keyword: extraction chromatography

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Determination of Normal Saturated- and Polycyclic Aromatic Hydrocarbons in the River Water of Bangladesh by Liquid-Liquid Extraction and Gas Chromatography

  • Mottaleb, M.A.;Sarma, D.K.;Sultana, S.;Husain, M.M.;Alam, S.M.M.;Salehuddin, S.M.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.1
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    • pp.99-105
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    • 2003
  • A liquid-liquid extraction followed by evaporative concentration method was used to determine the concentration of normal, or straight chain, saturated hydrocarbons (NSH) $(C_{10}\;to\;C_{24})$ and polycyclic aromatic hydrocarbons (PAH) here defined as: fluorene, anthracene, pyrene, chrysene and perylene, in the Buriganga River water of Bangladesh. Samples were collected from 5 and 25 cm depth of water at the southern, middle and northern parts of the river at Postogolla, Sadarghat and Sowarighat stations. Hydrocarbons were extracted from 450 mL of water into 75 mL n-hexane and then concentrated into 1 or 2 mL solution by evaporation. These solutions were analyzed by gas chromatography. The highest and lowest concentrations were determined as $257\;{\mu}gL^{-1}\;for\;C_{13}\;and \;0.24\;{\mu}g\;L^{-1}\;for\;C_{22}$ at 5 ㎝ depth of water, at the northern part of the Sowarighat and southern part of the Postogolla, respectively. This method could allow the analysis of water for $C_{22}$ as low as $0.24\;{\mu}g\;L^{-1}$.

Extraction and Separation of Protein-bound Polysaccharide by Lentinus edodes (표고버섯 배양액으로부터 단백다당류의 추출 및 정제 방법)

  • 박경숙;이별나
    • The Korean Journal of Food And Nutrition
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    • v.10 no.4
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    • pp.503-508
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    • 1997
  • The extraction and separation methods of protein-bound polysaccharides from the mycelium and culture broth of L. edodes were investigated. The use 2% solution of surface active agent, Triton X-100 was effective for extraction of the protein-bound polysaccharide from the mycelium. The extraction of the protein-bound polysaccharides from mycelium with hot water was achieved by 4 hours extraction at 10$0^{\circ}C$. For the separation and partial purification of the protein bound polysaccharides the column chromatography using DEAE-Cellulose, DEAE-Sephadex and Sephadex proved to be effective.

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Determination of capsaicinoids in red pepper powder using ultra high performance liquid chromatography (초고속 액체크로마토그래피를 이용한 고춧가루의 capsaicinoids 분석)

  • Namgung, Bae;Lee, Yunyeol;Ha, Jaeho
    • Analytical Science and Technology
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    • v.26 no.4
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    • pp.256-261
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    • 2013
  • The efficiency of the two extractions (refluxing extraction and heating-block extraction) was compared to develop the simple analytical method for the determination of capsaicinoids, including capsaicin and dihydrocapsaicin in red pepper powder. For the method development, the parameters, including particle size, extraction time and sample size, were evaluated using ultra high performance liquid chromatography (u-HPLC). It was found that the most effective extraction time of the refluxing extraction was 3 hr. The higher extraction efficiency was obtained with the fine particle of a mild red pepper powder, while the particle size did not affect the extraction efficiency in case of the hot red pepper powder. The higher extraction efficiency was obtained with the small size of sample taken because of the ratio of the large extracting solvent to sample amount. The extraction efficiency of the refluxing method was 3-9% higher than that of the heating-block method, however, the heating-block method could be applied to the determination of capsaicinoids in the red pepper powder for the purpose of quality control of the product.

Extraction and Purification of Bioactive Materials from Agaricus blazei Fruiting Bodies (아가리쿠스 버섯에서 생리활성물질의 추출 및 정제)

  • 최정우;류동열;김영기;홍억기;권명상;한진수
    • KSBB Journal
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    • v.15 no.3
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    • pp.293-298
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    • 2000
  • ${\beta}$-Glucan a kind of polysaccharide which is particularly abundant in Agaricus blazei is known as the bioactive materials especially anticancer agents. The process development of the isolation and the purification process of water soluble ${\beta}$-glucans from A. blazei was achieved. and the process operation variables were optimized. Crude polysaccharides (CR.PS) were obtained from A. blazei by hot water extraction filtration solvent precipitation dialysis and freeze drying. Neutral and acidic fraction of polysaccharides were separated from crude polysaccharides by ion chromatography and then high molecular weight and low molecular weight fraction were separated from neutral fraction by gel chromatography. Quantitative and qualitative analysis of each compounds were performed with FT-IR NMR spectroscopy. Based on these analysis the optimal conditions of temperatures operating time organic solvent volume for precipitation and dialysis time were determined.

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Application of Reversed-Phase Solid Phase Extraction for the HPLC Analysis of Microcystins in Water (다량 시료중 마이크로시스틴의 농축 및 분석)

  • Kim, Myeong-Hee;Kim, Tae-Seung;Kim, Tae-Keun;Park, Sun Ku
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.399-402
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    • 2000
  • To determine the concentrations of microcystins present in lake water or in tap water using high performance liquid chromatography, it is necessary to concentrate a large volume of water samples (about 20 L) into very small volume (0.1-0.3 mL). Concentration can be conveniently done when disc type solid phase extraction (SPE) apparatus is used. Using this apparatus we have investigated the recovery rates of three kinds of microcystins, RR, YR, LR. The recovery rates were relatively low and the reproducibilities were not good either. It is expected, however, that the appropriate selection of the disc conditioning and eluting solvents and reproducible reconcentration process after SPE will improve both the recovery rates and the reproducibilities.

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GC-MS Analysis of Ricinus communis, Pongamia pinnata, Datura metal, Azadirachta indica, Acalypha indica (leaf) Extract Using Methanol Extraction

  • J. Varshini premakumari;M. Job Gopinath
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.79-90
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    • 2023
  • Natural goods, especially therapeutic plants, are abundant in the World. Because they have the ability to provide all humanity with countless advantages as a source of medicines, medicinal plants are presently receiving more attention than ever. These plants' therapeutic efficacy is based on bioactive phytochemical components that have clear physiological effects on the human body. The drying process is crucial for the preparation of plant materials prior to extraction since freshly harvested plant materials include active enzymes that create active components, intermediates, and metabolic processes. Many of the phytoconstituents may be extracted using the semi-polar solvent methanol. The goal of the current work is to use the GC-MS gas chromatography- mass spectrometry technology to identify the phytochemicals and review their biological activity. In methanol leaf extract, 5 phytocompounds were found in Ricinus communis, 5 phytocompounds in Pongamia pinnata, 12 phytocompounds in Datura metal, 7 phytocompounds in Azadirachta indica, 11 phytocompounds in Acalypha indica.

Comparison of Preparation Methods for the Quantification of Ginsenosides in Raw Korean Ginseng

  • Hong, Hee-Do;Sim, Eun-Mi;Kim, Kyung-Tack;Rho, Jeong-Hae;Rhee, Young-Kyung;Cho, Chang-Won
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.565-569
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    • 2009
  • This study was conducted to evaluate the effects of different preparation methods on the recovery and quantification of ginsenosides in raw Korean ginseng (Panax ginseng C.A. Meyer). Eight major ginsenosides ($Rb_1$, $Rb_2$, $Rb_3$, Rc, Rd, Re, Rf, and $Rg_1$) were analyzed by high performance liquid chromatography (HPLC), after which the recovery and repeatability of the extraction of those ginsenosides using 3 different preparation methods were compared [A. direct extraction (DE) method, hot MeOH extraction/evaporation/direct dissolution; B. solid phase extraction (SPE) method, hot MeOH extraction/evaporation/dissolution/$C_{18}$ cartridge adsorption/MeOH elution; C. liquid-liquid extraction (LLE) method, hot MeOH extraction/evaporation/dissolution/n-BuOH fractionation]. Use of the DE method resulted in a significantly higher recovery of total ginsenosides than other methods and a relatively clear peak resolution. Use of the SPE and LLE methods resulted in clearer peak resolution, but lower ginsenoside recovery than the DE method. The LLE method showed the lowest ginsenoside recovery and repeatability among the 3 methods. Given that the DE method employed only extraction, evaporation, and a dissolution step (avoiding complicate and time consuming purification), this technique may be an effective method for the preparation and quantification of ginsenosides from raw Korean ginseng.

A Nucleoside with Lipid Peroxidation Inhibitory Activity from Agrocybe cylindracea. (버들송이로부터 분리한 Nucleoside계 화합물의 지질과산화 저해활성)

  • 이인경;윤봉식;유익동
    • Microbiology and Biotechnology Letters
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    • v.26 no.6
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    • pp.558-561
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    • 1998
  • In the screening for lipid peroxidation inhibitors from edible mushroom, Agrocybe cylindracea, a bioactive compound AG 8 was isolated. The AG 8 was purified from methanol extract of its fruit body by Diaion HP-20 column chromatography, ethyl acetate extraction, and silica gel column chromatography, consecutively. Based on various NMR studies including $^1$H irradiation and HMBC experiments, the AG 8 was identified as MTA, 5'-deoxy-5'-methylthioadenosine. This compound inhibited lipid peroxidation with an $IC_{50}$/ value of 3.2 $\mu\textrm{g}$/$m\ell$. The MTA was isolated for the first time from basidiomycetes.

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Analysis of lipopolysaccharides of Pasteurella multocida and several Gram-negative bacteria by gas chromatography on a capillary column (Gas chromatography의 capillary column을 이용한 Pasteurella multocida 및 기타 그람음성 세균의 lipopolysaccharide 분석)

  • Ryu, Hyo-ik;Kim, Chul-joong
    • Korean Journal of Veterinary Research
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    • v.40 no.1
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    • pp.72-80
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    • 2000
  • Lipopolysaccharides (LPS) of Pasteurella multocida (P multocida) and several Gram-negative bacterial pathogens were analyzed by methanolysis, trifluoroacetylation and gas chromatography (GC) on a fused-silica capillary column. The GC analysis indicated that LPS prepared from a strain of P multocida by phenol-water (PW) or trichloroacetic acid (TCA) extraction were quite different in chemical composition. However, LPS prepared from Salmonella enteritidis by the two extraction methods were very similar. PW-LPS extracts from different Pasteurella strains of a serotype had essentially identical GC patterns. Endotoxic LPS extracted from 16 different serotypes of P multocida by PW or by phenol-chloroform-petroleum ether procedures yielded chromatograms indicating similar composition of the fatty acid moieties but minor differences in carbohydrate content. When the chemical composition of endotoxic LPS extracted from several Gram-negative bacteria (P multocida, Pasteurella hacmolytica, Haemophilus somnus, Actinobacillus ligniersii, Brucella abortus, Treponema hyodysenteriae, Escherichia coli, Bacteriodes fragilis, Salmonella abortus equi and Salmonella enteritidis) were examined, each bacteria showed a unique GC pattern. The carbohydrate constituents in LPS of various Gram-negative bacteria were quite variable not only in the O-specific polysaccharides but also in the core polysaccharides. The LPS of closely related bacteria shared more fatty acid constituents with each other than with unrelated bacteria.

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Effects of Extraction Method on the Carnosine, Protein, and Iron Contents of Eel (Anguilla japonica) Extracts (뱀장어 (Anguilla japonica) 추출물 중의 Carnosine, 단백질 및 철분 함량에 미치는 추출방법의 영향)

  • Song, Ho-Soo;Lee, Keun-Tai;Kang, Ok-Ju
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.39 no.5
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    • pp.384-390
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    • 2006
  • To improve the extractability of carnosine and the levels of pro-oxidants such as iron in eel (Anguilla japonica) extracts, we examined the effects of extraction time, temperature, ion exchange chromatography and ultrafiltration (UF). The respective protein and total iron were reduced approximately 55 and 60% at 60$^{\circ}C$, 63 and 70% at 80$^{\circ}C$, 68 and 76% at 100$^{\circ}C$ and 82 and 48% with ion exchange chromatography, respectively, compared to the untreated extract. However, there was no significant difference in the carnosine levels in the eel extracts. Ultrafiltration reduced the protein content of the extract by 52% compared with the untreated extract. UF reduced the protein contents of the samples from 60, 80, and 100% heat treatment and ion exchange chromatography treatment by 27, 50, 46 and 47%, respectively. UF reduced the total iron contents of the identical four treatments by 14, 22, 23, and 43%, respectively, while UF increased the carnosine by 23, 17, 20, and 6%, respectively.