• 제목/요약/키워드: extraction solvent method

검색결과 599건 처리시간 0.023초

Gas chromatograph-mass selective detector를 이용한 식육 중 잔류농약의 동시분석 (Simultaneous detection method for pesticide residues in meat by gas chromatograph-mass selective detector)

  • 홍인석;최윤화;권택부;이정학
    • 한국동물위생학회지
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    • 제28권3호
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    • pp.285-294
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    • 2005
  • This study was conducted to investigate the extraction method for the determination of organochlorine, organophosphorus and synthetic pyrethroid pesticide residues in beef fat by gas chromatography-mass selective detector(GC-MSD). Twenty one pesticide residues in fat were determined using a simple and rapid procedure based on solid- phase extraction(SPE) clean-up cartridges with octadecyl $(C_{18})-bonded$ porous silica, florisil, $10\%$ deactivated florisil. a tandem $C_{18}$ and florisil and a tandem $C_{18}$ and $10\%$ deactivated florisil. Solvent-solvent extraction using acetonitrile was not satisfied to eliminate fat interference for pesticide residue analysis by GC-MSD, and the recoveries of the method in fat ranged from 16.2 to $57.3\%$ except DDT$(83.2\%)$. The recoveries of SPE methods using a tandem $C_{18}$ and Florisil was $59.6\~123.8\%$ except fenitrothion $(135.2\%)$. the SPE method was verified the satisfactory performance of pre-treatment for pesticide residues analysis in fat by GC-MSD. The efficiency of florisil deactivated with $10\%$ water has been not proved significantly on recoveries of pesticide residues in fat.

피크린 산에 의한 항히스타민제의 추출분광광도 정량 (Extraction Spectrophotometric Determination of Antihistamines with Picric Acid)

  • 신태용;엄동옥
    • 약학회지
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    • 제37권2호
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    • pp.119-123
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    • 1993
  • A spectrophotomertic method is proposed for the determination of antihistamines. The method is based on solvent extraction of the ion pair formed between antihistamines and colored picric acid into chloroform. The binding state of antihistamines-picric acid complexes were presumed by IR and $^{1}$H-NMR spectra as intermolecular hydrogen bonding. This method was applicable to the determination of antihistamines in the pharamaceutical preparations.

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Simultaneous determination of bisphenol A, chlorophenols and alkylphenols by solid-phase extraction and HPLC

  • Lee, Taejoon;Park, Keun-Young;Pyo, Dongjin
    • 분석과학
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    • 제30권1호
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    • pp.20-25
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    • 2017
  • An analytical method for determining potential endocrine disruptors (bisphenol A, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, p-t-butylphenol, p-pentylphenol, p-hexylphenol, p-t-octylphenol, p-heptylphenol, nonylphenol) by solid-phase extraction (SPE) and High Perfomance Liquid Chromatography(HPLC) equipped with fluorescence and variable wavelength detector has been developed. The SPE process for sample concentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of elution solvent and elution volume on the recoveries of the analytes were investigated with HPLC. Average recovery of >85% was achieved with 60mg sorbents using 5mL of methanol as elution solvent. Phenolic compounds in canned drinks, beverages and water samples were surveyed by this proposed method.

Microwave Energy를 이용한 오염토양에서 Phenol의 추출 (Extraction of Phenol from the Contaminated Soil Using Microwave Energy)

  • 이기환;이태호;김윤아
    • 한국환경과학회지
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    • 제12권4호
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    • pp.447-459
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    • 2003
  • This study was carried out to develop an efficient process far the elimination of phenol pollutant from soils. An microwave-assisted process (MAP) and a conventional Soxhlet extraction method (SEM) were employed to extract phenol from two types of soils. The effects of extraction methods, aged time of the spiked soil samples, extraction solvent and extraction time on the extraction performance were compared. Our results demonstrate that the recoveries from standard soil spiked were at least 10% higher fer MAP than these f3r the conventional Soxhlet. The extraction time by MAP requires significantly shelter time (1 min) than 15 h of the conventional Soxhlet. The recoveries from non-contaminated soil spiked with phenol were also almost identical f3r above results. The reduction of the extraction times with efficiency higher than that afforded by the conventional Soxhlet technique supports the suitability of the MAP method.

Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

  • Jung, Mi-Jin;Shin, Yeon-Jae;Oh, Se-Yeon;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • 제27권2호
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    • pp.231-236
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    • 2006
  • A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

가속화용매추출기를 이용한 히드록시프로필인산이전분의 프로필렌클로로히드린 분석방법에 관한 연구 (Analysis of Propylen Chlorohydrin in Hydroxypropyl Distarch Phosphate by Accelerated Solvent Extractor (ASE))

  • 이명자;신영민;정의한;최태진;정숙현;안원근
    • 한국식품영양과학회지
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    • 제31권4호
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    • pp.604-608
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    • 2002
  • 염소를 함유한 알콜류의 추출 및 분석은 일반적인 알콜류에 비해 비등점이 높아 휘발 또는 증류법을 적용하기 어렵고 특히 히드록시프로필치환전분 중 PCH의 추출은 전분입자와의 에멀션을 형성하므로 어려움이 있다. 따라서 용매를 가온, 가압하여 추출효율을 높이고, 전분의 물성적인 특성으로 인한 여과의 어려움을 해소할 수 있는 가속용매추출기 (ASE)를 사용하여 PCH 분석을 하였다. 온도 40~15$0^{\circ}C$의 변화에 따른 회수율을 측정한 결과 온도 상승에 따라 회수율이 증가하는 경향을 나타내어 12$0^{\circ}C$에서는 96.1%의 회수율을 나타내었다. 압력 변화에 따른 추출효율을 검토한 결과 1500 psi까지는 압력 상승에 따른 회수율의 증가가 뚜렷하여 93.6%였으나 이후에는 완만하게 증가하여 2500 psi에서는 96.1%로 나타났다. 추출용매(초산에틸, 메탄올, 아세톤, 디에틸에테르 및 핵산)에 따른 PCH의 회수율을 측정한 결과 아세톤, 디에틸에테르, 초산에틸은 94% 이상의 회수율을 나타내었고 메탄올 87.3%, 핵산 14.1%로 나타났다. RSD(%)는 초산에틸이 5.6%로 가장 우수하였다. ASE를 이용한 히드록시프로필치환 전분 중 PCH의 최적 추출조건은 온도, 12$0^{\circ}C$; 압력, 2500 psi; 추출용매, 초산에틸, static time, 50분; purge time, 300초; heating time, 5분; flush(%), 100 mL였으며, 이때 회수율은 96.1%이었다.

2차(次) 자원(資源)으로부터 습식방법(濕式方法)에 의한 인듐의 회수(回收) (Recovery of Indium from Secondary Resources by Hydrometallurgical Method)

  • 왕능운;이만승
    • 자원리싸이클링
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    • 제22권2호
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    • pp.3-10
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    • 2013
  • 인듐은 희유금속으로 주로 ITO제조에 사용된다. 본 총설에서는 인듐을 함유한 2차자원을 침출한 용액으로부터 인듐을 분리하기 위한 용매추출, 이온교환 및 석출법에 대한 공정 조건 및 장단점을 조사했다. 보통 정도의 산성용액에서 인듐의 추출제로 D2EHPA가 가장 많이 사용되고 있으며, 매우 강한 염산용액에서는 아민계 추출제가 사용된다. 일반적으로 이온교환수지의 인듐 흡착량이 낮으므로, 인듐의 농도가 낮은 경우에 한해 이온교환은 용매추출보다 장점이 있다.

Reprocessing of fluorination ash surrogate in the CARBOFLUOREX process

  • Boyarintsev, Alexander V.;Stepanov, Sergei I.;Chekmarev, Alexander M.;Tsivadze, Aslan Yu.
    • Nuclear Engineering and Technology
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    • 제52권1호
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    • pp.109-114
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    • 2020
  • This work presents the results of laboratory scale tests of the CARBOFLUOREX (CARBOnate FLUORide EXtraction) process - a novel technology for the recovery of U and Pu from the solid fluorides residue (fluorination ash) of Fluoride Volatility Method (FVM) reprocessing of spent nuclear fuel (SNF). To study the oxidative leaching of U from the fluorination ash (FA) by Na2CO3 or Na2CO3-H2O2 solutions followed by solvent extraction by methyltrioctylammonium carbonate in toluene and purification of U from the fission products (FPs) impurities we used a surrogate of FA consisting of UF4 or UO2F2, and FPs fluorides with stable isotopes of Ce, Zr, Sr, Ba, Cs, Fe, Cr, Ni, La, Nd, Pr, Sm. Purification factors of U from impurities at the solvent extraction refining stage reached the values of 104-105, and up to 106 upon the completion of the processing cycle. Obtained results showed a high efficiency of the CARBOFLUOREX process for recovery and separating of U from FPs contained in FA, which allows completing of the FVM cycle with recovery of U and Pu from hardly processed FA.

Application of the Microwave-assisted Process to the Fast Extraction of Isoflavone from the Waste Residue of the Soybeans

  • Hua, Li;Guoqin, Hu;Dan, Li
    • Bulletin of the Korean Chemical Society
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    • 제30권11호
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    • pp.2687-2690
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    • 2009
  • Due to the importance of isoflavone content in soybean extracts, the microwave-assisted process (MAP) was compared to the conventional extraction methods. For comparison of the three methods, all extraction parameters (solvent, sample to solvent ratio, temperature, etc.) were kept the same; the microwave extractor was operated at 187.5 W with an emission frequency of 2450 MHz under atmospheric pressure conditions and the extractions were carried out at 75 ${^{\circ}C}$ for 3 min while the conventional reflux was at 75 ${^{\circ}C}$ for 3 h. Total yield and crude isoflavone content were determined by ultraviolet spectrophotometric and compared with the three methods. Results indicated that the MAP was comparable to the conventional method in its capability to extract target compounds without causing any degradation; in addition it dramatically reduced the extraction time from 3 h to a few minutes, suggesting that it can be an alternative technique to the time-consuming conventional reflux method.

매립가스내 규소화합물류 검출을 위한 용매선택에 관한 연구 (Solvent Selection for the Detection of Siloxanes in Landfill gas)

  • 김낙주;최주미;지은정
    • 대한환경공학회지
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    • 제29권8호
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    • pp.915-921
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    • 2007
  • 본 연구는 매립가스내 siloxanes 측정의 기초 연구로서 국내 매립지를 대상으로 하여 용매흡수법으로서의 최적 용매를 선정하고자 수행하였으며, n-hexane, acetone 및 methanol을 흡수용매로 하여 각 용매의 siloxanes 검출 특성을 비교 분석하였다. 연구결과 표준물질의 GC분석에서 사용된 3가지 흡수용매 중 methanol이 용매와 silane 피크의 겹침현상이 발생하지 않아 분리능이 가장 우수하게 나타났다. 검출되는 siloxanes 농도는 흡수용매에 따라 최대 2.6배의 농도차를 보였으며, 포집유속과 포집 임핀저 단수에 대한 의존성에 대해서도 높은 것으로 나타났다. Methanol은 siloxanes 총 농도가 가장 높을 뿐만 아니라 휘발성이 적어 임핀저 단별 흡수에서도 가장 이상적인 형태를 보여주었으며, 가장 낮은 상대표준편차를 나타내 실험대상 매립지에 가장 적합한 것으로 나타났다. 그러나 용매의 적합성은 매립지의 쓰레기 성상, 매립이력에 따라 다를 수 있다고 판단된다.