• Title/Summary/Keyword: XAD

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Effective Purification of Ginsenosides from Cultured Wild Ginseng Roots, Red Ginseng, and White Ginseng with Macroporous Resins

  • Li, Huayue;Lee, Jae-Hwa;Ha, Jong-Myung
    • Journal of Microbiology and Biotechnology
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    • v.18 no.11
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    • pp.1789-1791
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    • 2008
  • This study was aimed (i) to develop an effective method for the purification of ginsenosides for industrial use and (ii) to compare the distribution of ginsenosides in cultured wild ginseng roots (adventitious root culture of Panax ginseng) with those of red ginseng (steamed ginseng) and white ginseng (air-dried ginseng). The crude extracts of cultured wild ginseng roots, red ginseng, and white ginseng were obtained by using a 75% ethanol extraction combined with ultrasonication. This was followed sequentially by AB-8 macroporous adsorption chromatography, Amberlite IRA 900 Cl anion-exchange chromatography, and Amberlite XAD16 adsorption chromatography for further purification. The contents of total ginsenosides were increased from 4.1%, 12.1%, and 11.3% in the crude extracts of cultured wild ginseng roots, red ginseng, and white ginseng to 79.4%, 71.7%, and 72.5% in the final products, respectively. HPLC analysis demonstrated that ginsenosides in cultured wild ginseng roots were distributed in a different ratio compared with red ginseng and white ginseng.

Part-Per-Trillion Level Determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water Samples (GC/MS-SIM 방법에 의한 수돗물 중 알킬페놀, 플로로페놀과 비스페놀 A의 ppt 정량)

  • Kim, Hyub
    • Environmental Analysis Health and Toxicology
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    • v.18 no.3
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    • pp.199-208
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    • 2003
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water samples. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the CC/MS SIM mode. The recoveries were 86.6 ∼ 105.2% (isoBOC derivatization) and 97.6∼484.5% (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol h for SIM were 0.001∼0.050 $\mu\textrm{g}$/1 (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/1 (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). When these methods were applied to tap water samples, the range of concentrations were 22.8∼31.3 ng/1 in 2,4-dichlorophenol, 28.6∼70.3 ng/1 in pentachlorophenol, 15.2∼17.4 ng/1 in t-butylphenol, 10.8∼13.2 ng/1 in t-octylphenol and 17.6∼36.3 ng/l in bisphenol A, respectively.

Identification of Higenamine nad its Metabolites in Rat by Gas Chromatography/Mass Spectrometry

  • Ryu, Jae-chun;Song, Yun-Seon;Kim, Myung-Soo;Cho, Jung-Hyuck;Yunchoi, Hye-Sook
    • Archives of Pharmacal Research
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    • v.16 no.3
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    • pp.213-218
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    • 1993
  • ($\pm$)-Higenamine is known as a cardiotonic principle of aconite root (root of Aconitum spp., Ranunculaceae). A simple and sensitive detection method for higenamine was developed by using gas chromatography-mass spectrometry (GC/MS). The recovery of higenamine after extraction and concentration with XAD-2 resin column was around 95% from rat biological fluids such as bile, plasma and urine. The limits of detection of higenamine in these biological fluids were approximately 0.1 ng/ml each. It has well been suggested that tetrahydroisoquinolines possessing catechol moiety such as higenamine should be subjected to the catechol-O-methyl transferase (COMT) activity in vivo. We detected two major peaks of presumed metabolites of higenamine in the total ion chromatogram obtained from the rat urine sample after the oral adminstration of ($\pm$)-higenamine. The scan mass spectrum of one of the metabolties coincided with those obtained from coclaurine $(C_6$-O-methyl higenamine) and those of the other metabolite are suggestive of isococlaurine $(C_7$-O-methyl higenamine).

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Constituents of Sanguisorba hakusanensis Leaves (산오이풀 잎의 성분)

  • Kwon, Won-Jun;Whang, Wan-Kyunn;Kim, Il-Hyuk
    • YAKHAK HOEJI
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    • v.40 no.3
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    • pp.262-272
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    • 1996
  • The constituents of Sanguisorba hakusanensis leaves (Rosaceae), of which the roots have been used as an astringent, hemostatics and antiphlogistics, were studied phytoche mically. From water fraction of the MeOH extract, gallic acid 3-O-${\beta}$-D-(6'-O-galloyl)-glucopyranoside(I), quercetin-3-O-${\beta$-D-galactopyranoside(II), quercetin-3-O-${\alpha}$-L-arabinopyranoside(III) and $2{\alpha},\;3{\beta},\;19{\alpha}$, 23-tetrahydroxyurs-12-en-28-oic acid 28-O-${\beta}$-D-glucopyranoside(IV) were isolated by column chromatographic separation using Amberlite XAD-2, ODS-gel and Sephadex LH-20. The structure of these compounds were elucidated by spectroscopic parameters of $^1H$-NMR, $^{13}C$-NMR, $^1H-^1H$ COSY, $^{13}C-^1H$ COSY, EI-Mass, FAB-Mass, IR, UV and by comparison with authentic samples.

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Isolation and Identification of Anthocyanins from Purple Sweet Potatoes

  • Lee, Lan-Sook;Chang, Eun-Ju;Rhim, Jong-Whan;Ko, Byoung-Seob;Park, Sang-Won
    • Preventive Nutrition and Food Science
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    • v.2 no.2
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    • pp.83-88
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    • 1997
  • Anthocyanin pigments of purple sweet potato roots (Ipomoea batatas L.) were extracted with 0.5% TFA (Trifluoroacetic acid) in 95% EtOh, and further isolated an purified by Amberlite XAD-7 and ODS column chromatography, and final preparative HPLC. Among nine anthocyanins isolated, the structure of three major anthocyanins were identified as 3-O-(6-O-trans-caffeyl)-2-O-(6-O-trans-caffeylglucopyranosyl)-$\beta$-D-glucopyranosyl-5-O-($\beta$-D-glucopyranosyl)-peonidin, 3-O-(6-O-trans-caffeyl)-2-O-(6-O-trans-feruloyl-glucopyranosyl)-$\beta$-D-glucopyranosyl-5-O-($\beta$-D-glucopyranosyl)-peonidin, and 3-O-(6-O-trans-caffeyl)-2-O-(6-O-p-hydroxylbenzoylglucopyranosyl)-$\beta$-D-glucopyranosyl)-peonidin, by using UV-visible absorption spectra, $^1$H-NMR and FAB-MS analysis.

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Combined Isobutoxycarbonylation and tert-Butyldimethylsilylation for the GC/MS-SIM Detection of Alkylphenols, Chlorophenols and Bisphenol A in Mackerel Samples

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.26 no.9
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    • pp.697-705
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    • 2003
  • The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 6$0^{\circ}C$ for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3∼150.6% and 93.8∼108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 $\mu$ g/kg and 0.010 $\mu$ g/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755∼0.9981 and 0.9908∼0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.

막분리(NF, UF)를 이용한 자연유기물(NOM) 제거에 관한 연구(II) - NF, UF 운전특성과 HAA생성능 제거 -

  • Song, Yang-Seok;Park, Yong-Hun;Jo, Yeong-Gwan;Jo, Jae-Won;Park, Don-Hui
    • 한국생물공학회:학술대회논문집
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    • 2003.04a
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    • pp.334-338
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    • 2003
  • In this study, We evaluated the removal efficiency of natural organic matters(NOM) in the Ultrafiltration(UF) and Nanofiltration(NF) membranes with molecular weight cutoff of 2500(GH), 8000(GM) and 250(HL), respectively. Filtration type was cross-flow filtration. The investigation result about raw water structure was hydrophobic 28%, hydrophilic 53% and transphilic 19%, in conjunction with XAD8/4 resin fractionation method. We were compared with UF(GM, GH) and NF(HL), in operation characteristic. In spite of poor MWCO, GM(8000Da) was superior than GH(2500Da), in the efficiency of total operation. It was showed the NF(HL) 80%, UF(GM) 50%, in the removing efficiency of HAAFP.

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Determination of Phthalates Compounds in the Ambient Atmosphere (II) - Evaluation of Experimental Artifacts and Sample Clean-up Procedures - (환경대기 중 프탈레이트 화합물의 농도 측정 (II) - 실험재료 전처리 및 시료정제과정 평가 -)

  • Park, Young-Hwa;Hwang, Yoon-Jung;Seo, Young-Kyo;Baek, Sung-Ok
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.5
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    • pp.455-460
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    • 2010
  • This study was carried out to find out any inherent problems occurring in the sampling and analytical procedures, and to suggest the relevant solutions to the problems. In addition, an optimal condition of clean-up process was developed, which was based on a method using silica glass column. As a result of experiments to test any artificial contamination of blank samples such as glassware and collection media, artifacts of DBP and DEHP appeared to be detected in various kinds of laboratory tools and apparatuses used in the sampling and analytical works. Therefore, it is necessary to investigate a degree of contamination before laboratory works by conducting a prior check any possible contaminations in all experimental tools and apparatus. It is also necessary to devise a method to avoid a tool, if possible, or to use a substitute of phthalate free. If the use of any plastic tool to cause contamination is inevitable, it should be properly corrected with a blank level, as is equally treated as the sample. The clean-up process demonstrated in this study can give us a significant benefit in terms of the quantity and quality of a target compound by GC/MS analysis.

Effect of Ambient Temperature on the Distribution of Atmospheric Concentrations of Polycyclic Aromatic Hydrocarbons in the Vapor and Particulate Phases (대기 중 다환방향족탄화수소의 기체-입자상 농도분포에 미치는 주변 온도의 영향)

  • 백성옥;최진수
    • Journal of Korean Society for Atmospheric Environment
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    • v.14 no.2
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    • pp.117-132
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    • 1998
  • The main purposes of this study are to investigate the distributional characteristics of polycyclic aromatic hydrocarbons (PAH) in the vapor and particulate phases in the ambient atmosphere, and to evaluate the effect of ambient temperature on the vapor-particle partitioning during the sampling period. A total of 64 samples were collected during a period of 1995 to 1996, using a medium-volume sampler with XAD-2 adsorbents and quartz fiber filters. Analyses of PAH were carried out using HPLC with UV and Fluorescence detections. In this study, a significant seasonal variation in the distributions was observed, reflecting the effect of ambient temperature on the vapor-particle partitioning of PAH. The relationship between the vapor-particle distributions of the 3 to 5 rings PAH and ambient temperature is considered to be well described using the Langmuir adsorption concept. The estimated empirical constants for each PAH in the relationship, particularly for the more volatile compounds, were also comparable with results from other studies. However, it is still difficult to accurately estimate the initial vapor-particle distribution of PAH in the ambient air, since it is not known to what extent the trapped vapours originated from the particles laden in the filter by being volatilized or from the air samples initially present in the vapour phase. The distribution factors for volatile PAH with 3 to 4 rings appeared to be comparable with those in the literature. It should be noted, however, that these distribution factors give information only about the distribution of PAH between the two phases under a specific sampling condition, and hence may provide only semi -quantitative information on the vapor-particle distributions in the atmosphere.

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전처리공정이 천연유기물질의 움집에 미치는 영향

  • 이주영;이석모
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 1997.10a
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    • pp.67-67
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    • 1997
  • 정수공정은 "원수 -1 침사지 1 전염소 -1 전오존 -1 침전지 1 여과지 1 후오존 1 GAC 4 후염소 1 가정수"로 이루어져 있으며 전처리 공정으로 염 소와 오존을 주입하게 되는데, 여기서 전염소 처리 공정으로 인해 잔류 유리염 소가 수중의 유기물질과 반웅하여 유해성 유기염소 화합물 (i.e.. Trihalomethane, Haloacetonitriles, Chlorophenol 등)을 생성하는 것으로 알려져 있다. 이러한 이유로 고도 정수처리 공정에서는 강한 산화력을 지닌 대체 산화 제로서 오존을 이용하고 있다. 전오존 처리공정은 OOC와 탁도 제거에 있어 응 집제 주입량을 감소시키는 것과 더불어 전오존 효과 (산화, 생분해 증대, 살균 등)를 얻을 수 있는 것으로 알려져 왔다. 그러나 낙동강과 같이 유기물이 많은 원수에 과다한 오존이 주입되면 수중 의 유기물이 저분자화 또는 응집이 어려운 오존 산화물로 변화하여 응집제의 소비가 많아지게 된다. 실제, 오존을 응집 효과에 대해서 pilot plant로 운전한 결과 전오존에 의해 입자성 물질의 제거 효율은 향상된 반면에 유기물 제거는 뚜렷한 효과를 볼 수 없었다고 보고되었다 (류, 1997). 본 연구에서는 물금 지역의 원수와 응집-침전 공정까지 거치는 각각의 처 리수에 대해서 전처리가 응집에 미치는 영향을 천연유기물질 (NOM)의 조성 변화로 파악하였다. 그 방법으로 천연유기물질 (NOM)을 XAD-1, -4 수지를 이 용하여 소수성 물질 (hydrophobic components)과 친수성 물질 (hydrophilic components)로 분리 및 농축하여 용존 유기물이 처리 과정에서 어떻게 변화하 는지를 조사하여 개선된 상수 처리 시스템을 설계하는데 기초 자료를 제공하고 수질 관리 분야에서도 적용하고자 하였다. 상수원수인 물금 지역의 소수성 물질(hydrophobic components)은 75~80%, 친수성 물질(hydrophilic components)은 30~33%정도의 분포를 보였고, 전염소 및 전오존 공정을 거친 처리수에서는 각각 62.2-62.8%, 43.9~49.0% 및 50~ 55%, 40~57% 정도의 분포를 보였다. 그리고 웅집-침전을 거친 처리수에서는 그 분포가 77~82%, 24-48%였다. 전주리 공정을 통하여 소수성 물질(byoghobic components)의 분포가 감 소하는 것을 볼 때 전염소 및 전오존 처리가 용존유기물의 응집에는 오히려 역 효과를 나타내는 것으로 판단된다. 것으로 판단된다.

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