• 제목/요약/키워드: extraction solvent method

검색결과 599건 처리시간 0.024초

MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석 (Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs)

  • 서계원;이재일;이채용;이정치
    • 한국식품위생안전성학회지
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    • 제18권2호
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    • pp.43-50
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    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

공동주택 건축내장재의 TVOC 방출량에 관한 예측모델 연구 (A Study on Predication model for TVOC Emissions of Finishing material in Apartment House)

  • 김형수;이경회
    • KIEAE Journal
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    • 제2권3호
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    • pp.55-62
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    • 2002
  • While cognition about an environment pollution becomes important recently, the intense pollution measures about an indoor air environment is required. In the case of building indoor environment, over 80% of modem people is living in building and these days an interest of building interior materials which becomes a reason for indoor environmental pollution in public house, office, is increasing. An experimental measurement method of this study is as follows. (1) American EPA TO-17, ASTMD5116-97, measurement method in VOCs experiment of Japanese closet industrial association (2) 2.4-DNPH cartridge method in HCHO experiment, based on American EPA TO-11 and measurement method of Japanese closet industrial association (3) standard compound is analyzed by using HPLC after solvent extraction process (4) paint and furniture are selected as measurement objects (5) we also made small chamber to grasp an emission characteristic of HCHO and VOCs and to get an environment-amicable forecast model through it, then we developed the model which can forecast emission rate by chamber experiment.

Simultaneous HPLC Analysis of Three Flavonoids in the Extracts of Artocarpus heterophyllus Heartwoods

  • Septama, Abdi Wira;Panichayupakaranant, Pharkphoom
    • Natural Product Sciences
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    • 제22권2호
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    • pp.77-81
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    • 2016
  • A reversed-phase high-performance liquid chromatographic method is described for the simultaneous determination of three antibacterial flavonoids, artocarpanone, artocarpin, and cycloartocarpin in ethyl acetate extracts from Artocarpus heterophyllus heartwoods. Separation was achieved using a TSK-gel ODS-80Tm column ($5{\mu}m$, $4.6{\times}150mm$) at $25^{\circ}C$ with a gradient elution system of methanol and water as follows: 0-8 min, 60:40; 8-27 min, 80:20; 27-35 min, 60:40, v/v, at a flow rate of 1 mL/min, and a quantitative UV detection at 285 nm. The method was validated by measuring the key parameters, including specificity, linearity, sensitivity, accuracy, repeatability and reproducibility. A high degree of specificity and sensitivity was achieved. The calibration curves for all three flavonoids showed good linearity with a coefficient of determinations ($R^2$) of ${\geq}0.9995$. The recoveries of the method were from 98-104%, with good reproducibility and repeatability (RSD values of less than 2%) were also achieved. Ethyl acetate was the best solvent for extraction of these three flavonoids using the heat reflux conditions for 1 h. This optimized sample preparation and HPLC method can be practically used for a routine standardization process of the extracts from the A. heterophyllus heartwoods.

A Novel Purification Process for Homoharringtonine from Celphalotaxus koreana

  • Sung, Ju-Li;Kim, Jin-Hyun
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2003년도 생물공학의 동향(XIII)
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    • pp.521-524
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    • 2003
  • An effective purification method was developed for producing Homoharringtonine (HHT), to guarantee high purity and yield from Cephalotaxus koreana. This process was a simple and efficient procedure, for the isolation and purification of HHT form the biomass of Cephalotaxus koreana, consisting of extract, adsorbent treatment, precipitation and followed by a chromatography. The extraction, adsorbent treatment and precipitation in pre-purification process allows for rapid and efficient separation of HHT from many compound and dramatically increases the yield and purity of crude HHT for HPLC purification steps compared to alternative processes. This purification processes serves to minimize solvent usage, size, and complexity of the operations for HHT purification.

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Gas Chromatography/Mass Spectrometry를 이용한 팔강약침액 성분에 대한 연구 (The Study on the Composition in Pharmacopunctures of Eight Principles by Gas Chromatography/Mass Spectrometry)

  • 김협;안병수
    • 대한약침학회지
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    • 제11권3호
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    • pp.79-91
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    • 2008
  • Objective: The purpose of this study was to investigate the composition for pharmacopunctures of eight principles hydrodistillation layer. Methods: The study was determined the hydrodistillation layer for pharmacopunctures of eight principles by hydrodistillation method. The effective components in hydrodistillation layer for pharmacopunctures of eight principles were extracted with ethyl ether or dichloromethane, and then analyzed by Gas Chromatography/Mass Spectrometry(GC/MS). Results: 1. Analyzed pharmacopunctures of eight principles by GC/MS, a lot of differences according to extraction solvent by each pharmacopunctures of eight principles and specific peak patterns were seen. 2. The main compound in pharmacopunctures of eight principles was a kind of hexaoxacyclohydrocarbon that has long hydrocarbon chain.

Methyl Orange에 의한 4급 Amine류의 Ion Pair 추출 흡광도 정량(I) - Cetyltrimenthylammonium bromide, Brethlium tosylate, Gallamine triethiodide 및 Thiamine의 정량 (Spectrophotometric Determination of Ion Pair Extraction of Quaternary Amines with Methyl Orange)

  • 최종환;김영수
    • 약학회지
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    • 제31권2호
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    • pp.45-51
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    • 1987
  • Methyl orange(MO) and cetyltrimethylammonium bromide(CTA) were mixed and added to 10ml of the buffer solution and then the solution was shaken for 5 minutes. The maximum absorption wavelength of the reaction product was 419nm. Dichloromethane was the best extracting solvent among the several organic solvents and the most suitable pH range was 2~8. When the CTA-MO calibration curve was made in the best experimental condition, the Lambert-Beer's law was obeyed in the range of CTA concentration of $1.5\times$$10^{-5}$~1.0$\times$$10^{-4}M$ by UV spectrophotometer. This method was possible to determine quaternary ammonium salts in the pharmaceutical preparations.

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Spectrophotometric Determination of Pipethanate Hydrochloride in Pharmaceutical Preparations with Methyl Orange

  • Chun, In-Koo;Chung, Hae-Soo;Lee, Min-Hwa;Chun, Bong-Kan
    • Journal of Pharmaceutical Investigation
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    • 제11권3호
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    • pp.1-13
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    • 1981
  • A new application of monoacidic dye is reported for the determination of pipethanate hydrochloride(PTH). The method is based on solvent extraction into chloroform of an ion-pair compound formed between methyl orange(MO) and PTH. PTH is determined by measuring absorbance of the extracts over the range of $2.0{\sim}12.0{\mu}g/ml$ at 420nm. Best accuracy can be obtained for solutions containing $3.0{\sim}8.0{\mu}g/ml$. The color was stable for at least 5 days. The molar absorptivity was $2.88\;{\times}\;10^4\;l,\;mol^{-1},\;cm^{-1}$. Molar ratio and continuous variation plots have a maximum at 0.5 mol fraction of MO, indicating a 1 : 1 MO-PTH ratio.

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기체크로마토그래피/질량분석기에 의한 수질시료 중 4-니트로톨루엔의 분석법 연구 (Analysis of 4-Nitrotoluene in Water by Gas Chromatography/Mass Spectrometry)

  • 이희경;권오승;류재천
    • Environmental Analysis Health and Toxicology
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    • 제15권1_2호
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    • pp.45-51
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    • 2000
  • Analytical method of 4-nitrotoluene (4-NT) in water was developed by 9as chromatography/mass selective detector/selected ion monitoring (GC/MSD/SIM). 4-NT was extracted with diethyl ether. Organic layer was washed with 5 % sodium chloride solution. The influence of solvent and evaporation condition on extraction of 4-NT were examined. The retention time of 4-NT peak was 7.72 min. Coefficient of variation (CV) of 4-NT (ng) within day and day-to-day was ranged from 7.0 to 14.6% and from 7.7 to 20.8%, respectively. Recovery of 4-NT was ranged from 84 to 109%, and detection limit of 4-H was lese than 1 ng/㎖.

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제조 방법을 달리한 갈색거저리 유충 탈지 분말의 물리화학적 특성 및 저장 안정성 (Physicochemical Characteristics and Oxidative Stabilities of Defatted Mealworm Powders under Different Manufacturing Conditions)

  • 손양주;황자영
    • 동아시아식생활학회지
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    • 제27권2호
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    • pp.194-203
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    • 2017
  • Mealworm, a type of edible insect, is a superior food material suitable for industrial products. In this study, four different defatted mealworm powders were prepared to determine proper manufacturing conditions. Solvent extraction method reduced lipid contents of mealworms more than pressed mealworms, and lowered lipid contents caused bright colors and good physicochemical properties for powders. In comparison, differences among milling machines used for making powders were strongly related with average size of particles. Meanwhile, the predicted shelf-life of defatted mealworm powders judged by accelerated experiments was 1 year or longer. To enhance shelf-life of mealworm powders, addition of tocopherol to mealworm powders at a concentration of 0.2% could intensify oxidative stability and microbial inhibition.

Isolation and Identification of Antimicrobial Substance from Canavalia gladiata

  • Lee, Hang-Young;Jeong, Heon-Sang
    • Food Science and Biotechnology
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    • 제14권2호
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    • pp.268-274
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    • 2005
  • Novel antimicrobial substance was isolated from seed coat of Canavalia gladiata by extraction with 75% methanol. Isolation and purification were conducted with solvent fractionation and chromatography on silica gel and sephadex LH-20 columns. Each fraction of antimicrobial activity was tested by paper disc method. Single compound was obtained from the 4th fraction of sephadex LH-20 column chromatography using chloroform/methanol (1:4, v/v), and identified as 3,4,5-trihydroxybenzoic acid methyl ester (methyl gallate) based on HPLC, GC/MS, FT-IR, $^1H$ NMR, and $^{13}C$ NMR analyses. This is the first report describing the presence of methyl gallate in C. gladiata.