• 제목/요약/키워드: extraction chromatography

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초임계 유체 추출법을 이용한 용담사간탕(龍膽瀉肝湯) 약침액(藥鍼液)의 정유(精油)성분에 대한 연구(硏究) (The Study on the Composition of Yongdamsagan-tang(龍膽瀉肝湯)'s Essential Oil Obtained by Supercritical Carbon Dioxide Extraction)

  • 이재은;김병우;임태진;김동희;;;권기록
    • 대한약침학회지
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    • 제11권1호
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    • pp.177-187
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    • 2008
  • Objectives : This study was performed to analyze the effective components of essential oil obtained from Yongdamsagantang, which has been efficacious against leukorrhea in gynecologic diseases. Methods : I obtained the essential oils of Yongdamsagan-tang by hydrodistillation extraction method and supercritical fluid extraction(SFE) method, and then I analyzed those by GC/MS(Gas Chromatography/Mass Spectrum). Results : 1. The optimum SFE(Supercritical Fluid Extraction) condition was obtained in the following experiment conditions: pressure 200atm, temperature $45^{\circ}C$, duration of extraction 25minutes. 2. With GC(Gas Chromatography) and GC/MS(Gas Chromato- graphy/Mass Spectrum) analysis, I identified 37 compounds in the Yongdamsagan-tang's essential oil obtained through the SFE method. The main compounds were as follows : 3-Methyl-but-2-enoic acid,2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H -pyrano[3,2-g]chromen-3-yl ester(49.81%), (Z)-6-Pentadecen-1 -ol(3.19%), (-)-Spathulenol(2.40%). 3. I identified 4 compounds in the Yongdamsagan-tang's essential oil obtained through the hydrodistillation method. The main compounds were as follows : 3-Methyl-but-2-enoic acid, 2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H-pyrano [3,2-g]chromen-3-yl ester(2.61%). 4. 3-Methy I-but-2-enoic acid, 2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H-pyrano[3,2-g] chromen-3-yl ester, all were identified in both the SFE method and the hydrodistillation method, but the others were not identified in common. 5. I also conducted an additional test in order to examine the essential oil's antimicrobial action against bacteria. Both MIC(Minimum Inhibitory Concentrations) and MBC(Minimum Bactericidal Concentrations) were $0.125mg/m{\ell}$ against N. meningitidis, however MIC and MBC were $1.0mg/m{\ell}$ in antimicrobial action against 12 different genera of bacteria.

Development of Quantitative Extraction Method of Amygdalin without Enzymatic Hydrolysis from Tonin(Persicae Semen) by High Performance Liquid Chromatography

  • Hwang, Eun-Young;Lee, Sang-Soo;Lee, Je-Hyun;Hong, Seon-Pyo
    • Archives of Pharmacal Research
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    • 제25권4호
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    • pp.453-456
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    • 2002
  • Tonin(Persicae Semen) is the herb medicine that contains amygdalin as a major ingredient. Amygdalin in water is decomposed into benzaldehyde, HCN, and glucose by emulsin, a hydrolysis enzyme in tonin. A useful and practical method for the optimum extraction condition of amygdalin without enzymatic hydrolysis is required. The extraction yield of amygdalin of natural formula to nin was 0.1 % from crude powders, 1.4% from small pieces, 3.5% from half pieces and 2.4% from whole pieces. The extraction yield of amygdalin of outer shell-eliminated to nin was 0.3% from crude powders, 1.4% from small pieces, and 3.5% from half pieces and whole pieces respectively. The extraction yield of amygdalin was most high when using the size larger than half.

Preparation of High Quality Safflower (Carthamus tinctorius L.) Seed Extract by High-Pressure Extraction Process

  • Seo, Il-Ho;Choi, Sang-Won
    • Preventive Nutrition and Food Science
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    • 제14권4호
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    • pp.373-377
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    • 2009
  • Safflower seed extract was prepared by a high-pressure extraction technology and its quality characteristics were compared to that of other conventional extraction techniques, such ultrasonic and reflux extractions. Safflower seeds were extracted with 80% aqueous ethanol by three above extraction methods, and further fractionated with Diaion HP-20 column chromatography to obtain a partially purified safflower seed extract (PPSSE). Among the three extraction techniques examined, the reflux extraction showed the higher yields of EtOH extract and PPE than the ultrasonic and high-pressure extractions. Levels of most phenolic compounds in the EtOH extract of safflower seed are higher in reflux and ultrasonic extractions than the high pressure extraction, but levels of two serotonin aglycones, N-(p-coumaroyl)serotonin (CS) and N-feruloylserotonin (FS), in PPSSE were higher in the high pressure extraction than the reflux and ultrasonic extractions. In addition, color values (L and a) of the PPSSE were higher in the high-pressure extraction than the reflux and ultrasonic extractions, although there were no significant differences in pH and UV maxima absorption spectra among three extraction techniques. These results indicate that the high-pressure extraction technology is a simple and effective extraction for preparation of a high quality of safflower seed extract containing CS and FS with anti-wrinkle activity.

A New Analytical Method for Erythromycin in Fish by Liquid Chromatography/Tandem Mass Spectrometry

  • Park, Mi-Jung;Park, Mi-Seon;Lee, Tae-Seek;Shin, Il-Shik
    • Food Science and Biotechnology
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    • 제17권3호
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    • pp.508-513
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    • 2008
  • Erythromycin has been used to treat Streptococosis, Edwardsiel1osis, Vibriosis, Bacterial enteritis in the cultured fish. In this study, a rapid and effective erythromycin analysis method with new sample treatment protocol and liquid chromatography/tandem mass spectrometry (LC/MS/MS) system for fish products was developed. For the erythromycin extraction from fish muscle, the solvent mixture composed of 0.2% meta-phosphoric acid and methanol (6:4) showed good recovery rate, and the optimum extraction solvent volume was 20 mL. Erythromycin detection using LC/MS/MS were carried out under electro spray ionization (ESI) positive condition and erythromycin mass value 576.2 and 157.9. And the detection limit of the established method was 0.005 mg/kg in fish products. The recovery rate of the developed method applied to the fish species were as following, olive flounder, $87.6{\pm}5.0%$; black rockfish, $87.2{\pm}6.4%$; eel, $85.2{\pm}4.8%$; and rainbow trout, $86.0{\pm}6.2%$. In the established method in this study, the correlation of coefficient values ($R^2$) of erythromycin calibration curve (n=11) was 0.9998.

LC/MS/MS를 이용한 유기인계 농약류의 최적 분석법 정립과 원·정수에서의 모니터링 (Development of Analytical Method and Monitoring of Organophosphorus Pesticides in the Raw Water and Clean Water by Liquid Chromatography-Tandem Mass Spectrometry)

  • 김경아;송미정;염훈식;손희종;이상원;최진택
    • 한국환경과학회지
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    • 제24권12호
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    • pp.1569-1582
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    • 2015
  • The analytical method for 16 organophosphorus pesticides was developed in this study. The 16 organophosphorus pesticides were analyzed by liquid chromatography-tandem mass spectrometry (LC/MS/MS) using on-line solid phase extraction (on-line SPE) with PLRP- S cartridge. Analysis of all analytes in the MS/MS was processed in the electrospray ioni-zation (ESI) positive mode. They are Azinphos ethyl, Chlorfenvinphos, Ethion, Famphur, Phosmet, Phosphamidon, Terbufos, Aspon, Chlorpyrifos-methyl, Crotoxyphos, Dichlofenthi-on, Dicrotophos, Fonofos, Thionazin, Dimethoate and Iprobenfos. Limits of detection (LODs) and Limits of quantification(LOQs) were obtained as 0.8~2.0 ng/L and 2.6~6.4 ng/L, respectively. All compounds were not detected at the 8 sampling points of the raw water and clean water.

식육중의 잔류 항생.항균제의 검정에 관한 연구(III) Macrolide계 항생물질인 Erythromycin과 Tylosin의 Gas Chromatography/Mass Spectrometry 동시분석 (A study on the determination of residual Antibiotics and Synthetic Antibacterial Agents in Meat(III) Simultaneous Gas Chromatography/Mass Spectrometry Analysis of Erythromycin and Tylosin)

  • 류재천;송윤선;양종순;서지원;김명수;박종세
    • 한국식품위생안전성학회지
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    • 제8권1호
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    • pp.17-23
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    • 1993
  • In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents n meat simultaneously, we studied a gas chromatogrphy-mass spectrometry (GC/MS) analysis. For a simultaneous analysis of macrolide antibiotics such as erythromycin and tylosin in meat, the homogenization with MeOH, defatting with n-hexane, extraction with CHCl3, elution with CHCl3 : MeOH=2:1 from Sep-Pak silica cartridge, acid gydrolysis, back extraction with CHCl3, and quantitation by selected ion monitoring(SIM) mode after trimethylsilyl derivatization were performed. The recoveries of erythromycin and tylosin (CV,%) at 10 ppm fortification level were 90.59(4.89) and 45.91(0.20) , and the detection limits of those were 0.02 and 2.0 $\mu\textrm{g}$/g beef, respectively. From these results, the developed analytical method using GC/MS-SIM mode allows excellent detection and quantitation of residual macrolide antibiotics in meats, using complementary method with bio-assay.

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Determination of Acrylamide in Foods by Solid Phase Microextraction-Gas Chromatography

  • Chen, Liangbi;Liu, Haizhu;Yu, Ping;Zhao, Jinyun;Chen, Xi
    • Food Science and Biotechnology
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    • 제18권4호
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    • pp.895-899
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    • 2009
  • A new approach for the determination of acrylamide (AM) in foods by solid phase microextraction-gas chromatography (SPME-GC) was established. AM was bromized and transformed to 2-bromoacrylamide (2-BAM). 2-BAM was then extracted by a commercial SPME fiber, $75-{\mu}m$ Car/PDMS fiber, for GC detection. The influence of extraction and desorption parameters such as extraction temperature and time, stirring rate, desorption temperature, and time were studied and optimized. The mass concentration was proportional to the peak area of 2-BPA from 1.0 to 8,000 ${\mu}g/L$. The detection limit of the SPME-GC for 2-BAM was found to be 0.1 ${\mu}g/L$, and the recoveries and relative standard deviations for different food samples were 74.5 to 102.0%, and 4.2 to 9.1%, respectively. The presented method was applied to the determination of AM in fried foods.

Profiling of Volatile Components Using Gas Chromatography-Mass Spectrometry in Commercial Pine Needle (Pinus densiflora S. and Z.) Powder

  • Kim, Joo-Shin;Chung, Hau-Yin
    • Preventive Nutrition and Food Science
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    • 제16권1호
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    • pp.45-54
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    • 2011
  • Volatile components in commercial pine needle (Pinus densiflora S. and Z.) powder were extracted using simultaneous steam distillation and a solvent extraction (SDE) apparatus, and were analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 230 compounds divided into 13 groups were identified, which included alcohols (42), ketones (39), aldehydes (32), terpenes (30), alkenes (17), esters (14), furans (14), benzenes (10), alkanes (8), napthalenes (7), acids (6), miscellaneous compounds (6), and phenols (5). Among the 230 compounds identified, 96 compounds were positively confirmed and quantified, and the rest of the compounds were tentatively identified. The major volatile components identified at relatively high levels were dodecanoic acid, hexadecanoic acid, hexanal, benzaldehyde, (Z)-3-hexen-1-ol, 1-penten-3-one, limonene, and $\beta$-caryophyllene oxide. Among the groups, terpenes accounted for 60.18% of the total concentration of all the volatile components. Some volatile components might account for the unique aroma and the biological activity of the sample.

Characteristic Impact Odorants of Changpo (Acorus calamus var. angustatus Bess) Root Essential Oil

  • Choi, Hyang-Sook
    • Food Science and Biotechnology
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    • 제14권4호
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    • pp.450-455
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    • 2005
  • This study was conducted to determine firstly the composition of the essential oil from fresh changpo (Acorus calamus var. angustatus Bess) roots quantitatively and qualitatively by use of two internal standards, and secondly volatile compounds which are primarily responsible for the aroma of changpo roots. Simultaneous steam distillation and extraction method was used for essential oil extraction, and aroma extract dilution analysis (AEDA) and sniffing test by gas chromatography/olfactometry (GC/O) were used to detect the characteristic impact odorants. According to the instrumental analysis of changpo root essential oil, cis, trans-famesol (47.56 mg/kg of fresh wt), octanoic acid (23.73 mg/kg of fresh wt), trans-2-dodecenal (20.28 mg/kg of fresh wt) and trans, trans-farnesol (13.81 mg/kg of fresh wt) were the most abundant compounds. Geranyl acetate, trans-nerolidol and trans, trans-farnesyl acetate were evaluated as the characteristic impact odorants of changpo roots from results of AEDA and sniffing test. Especially, geranyl acetate was considered as the most similar odor component to changpo roots by organoleptic evaluation with GC/O.

Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) Analysis of Liquid Crystalline Mixtures

  • Park, Gregory Hyung-Jin;Park, Ae-Na;Rho, Kyung-Rae;Shin, Jong-Ho;Kim, Yeong-Jeon;Jo, Sung-Chan;Oh, Weon-Sik
    • 한국자기공명학회논문지
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    • 제15권1호
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    • pp.14-24
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    • 2011
  • We have performed Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) analysis for liquid crystalline mixture and elucidated the structures of selected components by NMR spectra. Combining the results of one-dimensional 1H experiments as well as homonuclear and heteronuclear two-dimensional experiments, we could analyze the molecular structure of the liquid crystal singles whose structure had not been interpretable by mass spectrometry alone.