• 제목/요약/키워드: extraction chromatography

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GC-MS 기반 대사체학 기술을 응용한 참당귀의 산지비교분석 (Comparative Analysis of Cultivation Region of Angelica gigas Using a GC-MS-Based Metabolomics Approach)

  • 강귀보;임재윤
    • 한국약용작물학회지
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    • 제24권2호
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    • pp.93-100
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    • 2016
  • Background: A set of logical criteria that can accurately identify and verify the cultivation region of raw materials is a critical tool for the scientific management of traditional herbal medicine. Methods and Results: Volatile compounds were obtained from 19 and 32 samples of Angelica gigas Nakai cultivated in Korea and China, respectively, by using steam distillation extraction. The metabolites were identified using GC/MS by querying against the NIST reference library. Data binning was performed to normalize the number of variables used in statistical analysis. Multivariate statistical analyses, such as Principal Component Analysis (PCA), Partial Least Squares-Discriminant Analysis (PLS-DA), and Orthogonal Partial Least Squares-Discriminant Analysis (OPLS-DA) were performed using the SIMCA-P software. Significant variables with a Variable Importance in the Projection (VIP) score higher than 1.0 as obtained through OPLS-DA and those that resulted in p-values less than 0.05 through one-way ANOVA were selected to verify the marker compounds. Among the 19 variables extracted, styrene, ${\alpha}$-pinene, and ${\beta}$-terpinene were selected as markers to indicate the origin of A. gigas. Conclusions: The statistical model developed was suitable for determination of the geographical origin of A. gigas. The cultivation regions of six Korean and eight Chinese A. gigas. samples were predicted using the established OPLS-DA model and it was confirmed that 13 of the 14 samples were accurately classified.

Estimation of polycyclic aromatic hydrocarbons emission from sewage sludge of sewerage treatment plants in Korea

  • Kim, Dong-Hwan;Hwang, Jong-Seob;Lee, Min-Hee;Ok, Gon
    • 한국환경과학회지
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    • 제12권11호
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    • pp.1167-1171
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    • 2003
  • Polycyclic aromatic hydrocarbons (PAHs) are an important group of organic contaminants present in sewage sludge, due to their persistence, toxic, bioaccumulative and long range transfer. These characters make themselves as Persistent Organic Pollutants(POPs) in Long Range Transboundary Air Pollutions convention(LRTAP) of Europe. A method of the gas chromatographicmass spectrometric (GCMS) determination of PAHs present in sewage sludge was developed and applied to analyzed samples from five sewerage treatment plants (SWTPs), having different treatment types. PAHs were extracted from freeze-dried samples by toluene 16 hours in a soxhlet extraction system. The sludge extracts were cleaned-up by an activated silica gel column chromatography. The sum of the 16 US Environmental Protection Agency PAHs sewage sludge samples varied from 2.44 to 4.82 $\mu\textrm{g}$/g. Concentration of emission carcinogen PAHs(PAHcarc), such as Benzo(a)anthracene, Benzo(b)f1uoranthene, Benzo(k)f1uoranthene, Benzo(a)pyrene, Dibenzo(a,h)anthracene and Indeno( 1,2,3-cd)pyrene ranged from 0.62 to 1.03 $\mu\textrm{g}$/g. The total amount of PAHs emission from sewage sludge in Korea was calculated as a top-down approach. PAHs and $\Sigma$PAHcarc from sewage treatment plants had emitted to environment by several pathway. The highest amount of emission to the environment was remarked in the ocean dumping(PAHs and $\Sigma$PAHcarc emissions were 1155.95 kg/year and 5040.32 kg/year, respectively).

참당귀(Angelica gigas Nakai) 중 Decursin 및 Decursinol Angelate의 분리 및 정제 (Isolation and Purification of Decursin and Decursinol Angelate in Angelica gigas Nakai)

  • 김강민;정재연;황성우;김묘정;강재선
    • 한국식품영양과학회지
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    • 제38권5호
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    • pp.653-656
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    • 2009
  • 생약재로 사용 중인 Angelica gigas Nakai의 decursin 및 decursinol angelate를 60% ethanol로 최종적으로 추출 후 recycling HPLC 및 HPLC/MS에 의해 각각을 분리하였다. 60% ethanol로 $-20^{\circ}C$에서 추출하였을 경우 95% 순도의 decursin 및 decursinol angelate를 얻을 수 있었고 10번 이상의 recycle를 통해서 순수한 decursin 및 decursinol angelate를 분리할 수 있었다. 분리한 decursin 및 decursinol angelate를 HPLC/MS를 통해 분자량을 확인하였을 경우 m/z=329($[M+H]^+$) 및 m/z=351($[M+Na]^+$)과 같은 결과를 얻을 수 있었다. 이 분리 방법을 통해 decursin 및 decursinol angelate를 통한 의약품 및 식품 등에 관한 여러 연구에 있어 두 물질 각각에 대한 약리학적 효과를 도출하는데 기여할 것이며, 물질표준화에 기여할 것으로 사료된다.

성견에서 임프란트 매식시 골형성단백 사용에 따른 골재생에 관한 연구 (A STUDY OF EFFECTS OF BONE MORPHOGENETIC PROTEIN BONE REGENERATION OF IMPLANTS IN DOGS)

  • 조진희;방몽숙;이종호
    • 대한치과보철학회지
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    • 제32권4호
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    • pp.593-607
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    • 1994
  • The purpose of this study is to evaluate the effect of the bone morphogenetic protein, bone matrix gelatin and collagen matrix on the amount and shape of generating new bone adjacent to the implant. Implants were inserted in the mandible of adult dogs at 2 months after teeth extraction. Artificial bony defects, 3mm in width and 4mm in depth were made at the mesial and distal side of implant. Experimental groups were divided into three groups ; Group 1 : Defects filled with collagen matrix and bone morphogenetic protein, Group 2 : Defects filled with bone matrix gelatin. Control group : Defects filled with only collagen matrix. After implantation, the animals were sacrificed at 1,3,5 and 10 weeks for light microscopic examination. For the fluorescent microscopic examination. each tertracycline Hcl and calcein were injected at 1, 3, 5, 8 and 10 weeks after implantation. The results obtained were as follows : 1. The molecular weight of bovine BMP was about 18,100 by hydroxyapatite chromatography. 2. Osseointegration was observed in experimental groups 1 & 2, and BMG and BMP had an excellent bone forming capability as a filling materials to the repair of the bone defects. 3. The degree of healing of bone defect area, the experimental group 1 showed more prominent bone formation than control group, and the control group showed fibrous connective tissue between the implant and the bone. 4. In the fluorescent microscopic findings, bone remodelling was observed regenerative lamellar bone at defect area in experimental group 1, and partial remodelling in experimental group 2, In the control group, fibrous connective tissue was observed between the implant and bone surface and sign of remodelling was not apperaed. Above results suggest that BMP has rapid osteoinductive property and can be used clinically as a bone substitute on bone defects around implants.

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알파분광법과 중성자방사화분석법에 의한 극미량의 악티늄계원소 (Am, Pu, Th, U)분석연구 (Determination of trace actinide (Am, Pu, Th, U) using alpha spectrometry and neutron activation analysis)

  • 윤윤열;조수영;이길용;김용제;이명호
    • 분석과학
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    • 제17권4호
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    • pp.302-307
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    • 2004
  • 환경시료중의 극미량의 악티늄계 동위원소들을 분석하기는 무척 어렵다. 이들 원소들은 개별 분리하는 작업이 필요하며, 알파분광법으로 분석한 어떤 핵종들은 검출감도도 높은 편이다. 이런 극미량의 악티늄계 동위원소들을 분석하기 위해 용매추출법이 결합된 TRU-Spec 이온교환수지와 음이온 교환수지를 사용하여 악티늄계 원소들을 분리한 후 알파분광법으로 검출하였다. 그리고 U과 Th의 검출한계를 낮추기 위해 중성자방사화분석법을 적용하였다. 중성자방사화분석법을 적용하기 위한 바탕물질로 고순도 V foil을 사용하여 검출감도를 10배 향상시킬 수 있었으며, 이 분석법을 표준시료인 NIST-4354, IAEA-368 퇴적물 시료에 적용한 결과 표준값과 10% 이내에서 잘 일치하였다.

Simultaneous Analysis of Bioactive Metabolites from Rehmannia glutinosa by HPLC-DAD-MS/MS

  • Won, Tae-Hyung;Ryu, Sung-Kwang;Kang, Sam-Sik;Shin, Jong-Heon
    • Natural Product Sciences
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    • 제16권2호
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    • pp.116-122
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    • 2010
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of five representative metabolites of the iridoid and phenolic classes from Rehmannia glutinosa. The optimal chromatographic conditions were obtained on an ODS column (5 mm, $4.6{\times}250\;mm$) with the column temperature at $25^{\circ}C$. The mobile phase was composed of water and acetonitrile using a gradient elution with the flow rate 0.3 mL/min. Detection wavelength was set at 205 nm. All calibration curves showed good linear regression ($r^2$ > 0.997) within test ranges. Limits of detection (LOD) and quantitation (LOQ) values were lower than 0.123 and $0.373\;{\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.09 - 0.76% and 0.16 - 1.41%, respectively, and the overall recoveries of 99.03 - 102.67% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytic method. The verified method was successfully applied to the quantitative determination of five representative metabolites in twenty-one commercial Rehmannia glutinosa samples from different markets in Korea and China. The analytical results showed that the contents of the five analytes vary significantly with sources.

Role of Glutathione Conjugation in 1-Bromobutane-induced Immunotoxicity in Mice

  • Lee, Sang-Kyu;Lee, Dong-Ju;Jeon, Tae-Won;Ko, Gyu-Sub;Yoo, Se-Hyun;Ha, Hyun-Woo;Kang, Mi-Jeong;Kang, Won-Ku;Kim, Sang-Kyum;Jeong, Tae-Cheon
    • Toxicological Research
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    • 제26권2호
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    • pp.101-108
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    • 2010
  • Halogenated organic compounds, such as 1-bromobutane (1-BB), have been used as cleaning agents, agents for chemical syntheses or extraction solvents in workplace. In the present study, immunotoxic effects of 1-BB and its conjugation with glutathione (GSH) were investigated in female BALB/c mice. Animals were treated orally with 1-BB at 375, 750 and 1500 mg/kg in corn oil once for dose response or treated orally with 1-BB at 1500 mg/kg for 6, 12, 24 and 48 hr for time course. S-Butyl GSH was identified in spleen by liquid chromatography-electrospray ionization tandem mass spectrometry. Splenic GSH levels were significantly reduced by single treatment with 1-BB. S-Butyl GSH conjugates were detected in spleen from 6 hr after treatment. Oral 1-BB significantly suppressed the antibody response to a T-dependent antigen and the production of splenic intracellular interlukin-2 in response to Con A. Our present results suggest that 1-BB could cause immunotoxicity as well as reduction of splenic GSH content, due to the formation of GSH conjugates in mice. The present results would be useful to understand molecular toxic mechanism of low molecular weight haloalkanes and to develop biological markers for exposure to haloalkanes.

차에 함유된 methylxanthin류, catechin류 및 theaflavin류의 HPLC에 의한 동시분석법 (Analytical Method for Methylxanthin, Catechin, and Theaflavin Determinations in Korean Commercial Teas by HPLC)

  • 김수연;소궤신행;한재숙;이갑랑
    • 한국식품과학회지
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    • 제38권1호
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    • pp.5-9
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    • 2006
  • 본 연구는 차에 함유되어 있는 특유의 정미성분으로 methylxantin류, catechin류 및 theaflavin류의 총 13종의 화합물을 HPLC를 이용한 동시분석법을 확립함과 동시에 이 분석법을 이용하여 한국에서 사판되고 있는 녹차, 홍차 및 우롱차에 함유되어 있는 주요 성분을 분석하였으며 그 결과는 다음과 같다. HPLC분석조건은 역상(ODS)column을 이용하여 acetonitrile: 20 mM 인산완충액의 solvent 중 acetonitrile의 농도를 처음 단계 7%에서 최종 40%까지 단계적으로 변화시켜 분당 1mL씩 용출시켜 분석하였다. Column 온도는 효과적으로 각 성분을 분리시키기 위하여 정확하게 $30^{\circ}C$로 설정하였으며 파장은 270 nm에서 분석하였다. 또한 차에 함유되어 있는 methylxantin류, catechin류 및 theaflavin류의 총 13종의 화합물을 분석한 결과, 한 시료당 90분이 소요되었으며 재현성과 정량성이 뛰어나 13종의 화합물이 완전하게 분리되었다. 시판 녹차, 홍차, 우롱차를 분석한 결과, 녹차와 우롱차는 2종류의 methylxantin류와 7종류의 catechin류는 검출되었으나 홍차에서 검출된 4종류의 theaflavin류는 전혀 나타나지 않았다. 이러한 결과는 차의 품질 관리 및 소비자의 차 선택에 있어 중요한 기초자료가 될 것으로 사료된다.

A comparative study of Sargassum horneri Korea and China strains collected along the coast of Jeju Island South Korea: its components and bioactive properties

  • Kim, Hyun-Soo;Sanjeewa, K.K. Asanka;Fernando, I.P. Shanura;Ryu, BoMi;Yang, Hey-Won;Ahn, Ginnae;Kang, Min Cheol;Heo, Soo-Jin;Je, Jun-Geon;Jeon, You-Jin
    • ALGAE
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    • 제33권4호
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    • pp.341-349
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    • 2018
  • Sargassum horneri is edible brown seaweed abundant along the coasts of Jeju Island, South Korea. In addition to the native S. horneri population, a large amount of S. horneri has been found to invade Jeju Island from the east coast of China. Thus, S. horneri of both Korea (SK) and China (SC) strains now inhabits along with the shore of Jeju Island and have become a threat to the coastal biodiversity. However, they could be used in obtaining functional ingredients for industrial level applications provided an optimized cost effective strategy. In the present study, we compared SK and SC strains for the extraction efficiency, components, antioxidant, and anti-inflammatory properties of 80% methanolic extracts and their partially purified fractions. According to the results, two strains indicated similar bioactive properties such as DPPH and alkyl radical scavenging activity as well as anti-inflammatory activities on lipopolysaccharide-stimulated RAW 264.7 cells. The yield of 80% methanol extract from SC was higher than SK. However, the yields of the ethyl acetate and chloroform fractions from SK were higher than those of SC strain. The major peaks in the high-performance liquid chromatography chromatograms, which was identified as Apo-9 fucoxanthinone, indicated that both methanolic extracts of SK and SC contains major target peaks but with different amounts. This study might be useful for developing functional materials from SC and SK in future.

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • 고려인삼학회:학술대회논문집
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    • 고려인삼학회 2002년도 학술대회지
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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