• 제목/요약/키워드: Accelerated solvent extraction

검색결과 20건 처리시간 0.034초

농산물의 잔류농약분석을 위한 가속용매추출 (Accelerated Solvent Extraction) 방법의 이용 (Use of Accelerated Solvent Extraction Method for Determination of Residual Pesticides in Agricultural Products)

  • 이성우;서혜영;한병재;정양모;김준형;노기미;김경수
    • Applied Biological Chemistry
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    • 제47권2호
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    • pp.228-237
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    • 2004
  • 농약성분 분석에 있어서 시료 전처리시간을 단축할 수 있는 분석방법을 개발하기 위해 농산물 중에 잔류하고 있는 잔류농약성분을 대상으로 ASE(accelerated solvent extraction) 방법을 활용한 자동화된 전처리 방법을 검토하였다. ASE 추출조건은 preheat 1 min, heat 5 min, static 1 min, solvent flush% 60 vol, nitrogen purge 60 sec, cycle 4, pressure 1500 psi, temperature $100^{\circ}C$를 선택하였다. 이 분석조건과 n-hexane:acetone(4 : 1, v/v)를 추출용매로 사용하였을 때, ASE 추출과 정제능력은 solvent extraction 방법과 유의적인 차이를 보이지 않았고, 추출 용매의 감소는 추출산물의 재현성에 큰 영향을 미치지 않았다. ASE 방법은 잔류농약 분석 시 소요되는 유기용매의 양을 감소하고 추출과 정제를 동시에 수행함으로써 동결건조 시간을 제외한 전처리 시간이 단축되어 분석비용 또한 solvent extraction에 비해 감소시킬 수 있었다.

Analytical Method for Dioxin and Organo-Chlorinated Compounds: (Ⅱ) Comparison and Extraction Methods of Dioxins from XAD-2 Adsorbent

  • 양정수;이성광;박영훈;이대운
    • Bulletin of the Korean Chemical Society
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    • 제20권6호
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    • pp.689-695
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    • 1999
  • Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins(PCDDs) from the XAD-2 resin which was used to adsorb PCDDs in the atmosphere. XAD-2 resin spiked with five PCDDs was chosen as a sample. The optimum conditions for the extraction of PCDDs by SFE were turned out to be the use of CO2 modified with 10% toluene at 100 ℃ and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDDs ranging from 68 to 98%. The ultrasonic extraction of PCDDs from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDDs for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of tem-perature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was n-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDDs ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations.

ASE와 SPMDs를 이용한 퇴적물중 PCDD/Fs의 전처리법 개발 (Pretreatment Method Development of PCDD/Fs in Sediment Using ASE and SPMDs)

  • 천만영
    • Environmental Analysis Health and Toxicology
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    • 제22권1호
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    • pp.49-55
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    • 2007
  • Three kind of ASE (Accelerated Solvent Extraction) and SPMDs (Semi-Permeable Membrane Devices) combined methods (ASE-SPMDs, ASE-accelerated SPMDs and SPMDs without extraction) and general Soxhlet-GPC were compared each other for the analysis of PCDD/FS in sediment. The average recovery rate of three types ASE and SPMDs combined methods (108.1%) were higher than that of the Soxhlet-GPC (79.5%) for three samples in each method using surrogate internal standards. The average coefficient of variation (10%, $2.1{\sim}25.2%$) for each congener of PCDD/Fs shows the reasonable results. Total PCDD/Fs concentrations after SPMDs without extraction were quite low, but those after ASE-SPMDs and ASE-accelerated SPMDs methods were close to the Soxhlet-GPC. Thus, the ASE-SPMDs and ASE-accelerated SPMDs methods are considered as the excellent pre-treatments method because they need less solvent and time without quality degradation.

대기 중 다환방향조탄화수소류의 분석 방법간 비교연구 (A Comparative Study on the Analytical Methods of Polycyclic Aromatic Hydrocarbons in the Atmosphere)

  • 박찬구;김민영;정동균;모세영
    • 한국대기환경학회지
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    • 제16권6호
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    • pp.595-606
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    • 2000
  • In order to compare analytical conditions for measuring PAHs(polycyclic aromatic hydrocarbons) in ambient air, a series of experiment were conducted using three different types of extraction methods that include:(1) accelerated solvent extraction (ASE), (2) soxhlet, and (3) sonification methods. Efficiency and relevant analytixal parameters for each of these methods were examined on five different types of solvents that include:(1) 10% diethyl ether in n-hexane(v/v), (2) dichloromethane, (3)cyclohexane.(4) toluene, and (5) Benzene: ethanol (4:1). Comparison of extraction efficiency for various combinations between methods and solvents was made through an application of both internal and external standard calibration techniques. The extraction efficiency tests, when checked using both internal and external standards, allowed us to derive meaningful comparison among different techniques and among solvents.

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Optimization and Bioassay Guided Comparative Techniques for Efficient Extraction of Lutein Esters from Tagetes erecta (Var. Pusa Narangi Genda) Flowers

  • Kawar Lal Dabodhia;Brijesh Tripathi;Narendra Pal Lamba;Manmohan Singh Chauhan;Rohit Bhatia;Vivek Mishra
    • Mass Spectrometry Letters
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    • 제15권1호
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    • pp.40-48
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    • 2024
  • Capacity of the analytical/quantitative evaluation techniques to satisfy both qualitative and quantitative considerations for effective extraction of marigold oleoresins/xanthophylls and their potential as anti-mycotic and antioxidant activity was assessed. Accelerated solvent extraction (ASE), Soxhlet extraction (SE), Supercritical fluid extraction (SCFE), Cold extraction (CE), and ultrasonically assisted extraction (USE) techniques were evaluated for extraction of oleoresin/xanthophyll content from Tagetes erecta (Var. Pusa Narangi Genda) with respect to solvent consumption, extraction time, reproducibility, and yield. Followed by the antifungal and antioxidant activity evaluation. The overall yield of Tagetes oleoresin was higher in ASE (64.5 g/kg) followed by SE (57.3 g/kg), USE (50.7 g/kg), SCFE (45.3 g/kg) and CE (31.6 g/kg). The lutein esters represented more than 80% of the constituents. Further, xanthophyll/ lutein content in oleoresin was found to be quite higher in HPLC (r2 = 0.996) analysis than in the AOAC recommended UV spectrophotometer analysis. The oleoresin exhibited moderate antioxidant activity (DPPH assay) and antifungal activity against three phytopathogenic fungi. Based on the various parameters, the reproducibility of ASE was better (0.3-8.0%) than that of SE (0.5-12.9%), SCFE (0.2-9.4%), USE (0.3-12.4%) and CE (0.8-15.3%). ASE with (RSD 1.6%) is preferred being faster, reproducible, uses less solvent, robust and automation allows sequential extraction of the sample in less time.

ASE 및 SPE 복합정제법을 이용한 친환경농업토양의 다성분잔류농약 분석 (Pesticide Multiresidues Analysis of Environmental-friendly Agricultural Soils by the Complex Cleanup Method of Accelerated Solvent Extraction (ASE) and Solid Phase Extraction (SPE))

  • 문경미;박진우;이영근;최영환
    • 농업생명과학연구
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    • 제45권5호
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    • pp.73-80
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    • 2011
  • 국내의 친환경농산물과 토양에서 자주 검출되는 농약 50성분을 선정하고, 경남지역의 친환경농산물 재배농지의 토양시료 40점을 대상으로, 가속용매추출법(accelerated solvent extraction)과 고상추출법(solid-phase extraction)의 복합처리법으로 정제하고 GC/ECD/NPD, HPLC/UV/FL, GC/MSD 및 HPLC/MSD를 이용한 분석법을 적용하여 잔류농약의 잔류실태를 조사하였다. 적용한 분석법에 의한 농약 회수율은 72~118%의 범위로 평균 95.5%이었고, CV(%)값 평균은 3.0%로 나타났다. 토양 40점 중 잔류농약 검출은 21점에서 20성분이 검출되었으며 검출토양의 농약별평균 검출량은 endosulfan 0.035, ethoprophos 0.043, chlorpyrifos 0.020, chlorfenapyr 0.023, flufenoxuron 0.047, fenvalerate 0.070, cypermethrin 0.266, lufenuron 0.016, bifenthrin 0.022, fenobucarb/BPMC 0.025, difenoconazole 0.043, fenarimol 0.059, kresoxim-methyl 0.020, tetraconazole 0.026, isoprothiolane 0.039, iprobenfos 0.017, nuarimol 0.014, fluquinconazole 0.156, tebuconazole 0.047 및 oxadiazon이 0.045 mg/kg으로 나타나서 친환경재배농지의 토양환경기준에 잔류농약의 설정이 시급하다고 판단되었다.

반응표면분석법을 사용한 가속 용매 추출에 의한 홍삼 지표성분의 추출 최적화 (Optimization of Extraction of Marker Compounds from Red Ginsengs by Accelerated Solvent Extraction Using Response Surface Methodology)

  • 김은옥;서구량;엄병헌
    • 한국식품영양과학회지
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    • 제45권8호
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    • pp.1162-1169
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    • 2016
  • 본 연구에서는 기능성 홍삼 엑기스 제조를 위해 추출용매, 압력, 온도, 추출시간을 조절하여 가속 용매 추출한 후 기능성 홍삼제품의 지표성분인 진세노사이드 함량, 총페놀화합물 및 벤조피렌 함량 등을 조사하였다. 홍삼 가속 용매 추출 최적화를 위한 독립변수 선택을 위해 에탄올 농도, 압력, 온도 및 추출시간에 따른 기능성 홍삼제품의 지표성분인 진세노사이드 Rb1, Rg1 및 Rg3(20S) 함량의 합을 분석하여 진세노사이드 추출에 가장 최적의 용매를 50% 에탄올로 하고, 영향이 다소 작았던 요인인 압력을 2,500 psi로 설정하였으며, 온도와 추출시간을 독립변수로 설정하였다. 추출 온도 및 시간을 독립변수로 하여 고온고압 처리한 홍삼의 진세노사이드 Rb1, Rg1 및 Rg3(20S) 함량의 합, 총 페놀성 화합물 및 벤조피렌 함량을 측정한 결과, 벤조피렌이 검출되지 않는 조건에서 진세노사이드 Rb1, Rg1 및 Rg3(20S)의 함량 합이 최적화된 조건은 $158^{\circ}C$, 20분임을 확인할 수 있었다. 최적화된 조건에서의 가속 용매 추출 시 초음파 및 환류냉각 추출에 비해 적은 용매로 단시간 추출하면서 진세노사이드 Rb1, Rg1 및 Rg3(20S) 함량 합 및 총폴리페놀 함량이 각각 1.5~2배 및 2.2~5배 높게 추출할 수 있어 효율적인 추출방법이 될 것으로 생각된다.

Extraction of Hemicellulosic Sugar and Acetic Acid from Different Wood Species with Pressurized Dilute Acid Pretreatment

  • Um, Byung-Hwan;Park, Seong-Jik
    • Journal of the Korean Wood Science and Technology
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    • 제42권2호
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    • pp.172-182
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    • 2014
  • Extraction is a necessary element in the bioconversion of lignocellulosics to fuels and chemicals. Although various forms of chemical pretreatment of cellulosic materials have been proposed, their effectiveness varies depending on the treatment conditions and substrate. In this study, mixed hardwood (MH) and loblolly pine (LP) were pretreated with dilute acid in a 100 mL accelerated solvent extraction (ASE) at the predetermined optimal conditions: temperature: $170^{\circ}C$, acid concentration: 0.5% (w/v), and reaction time: 2~64 min. This method was highly effective for extracting the hemicellulose fraction. Total xmg (defined as the sum of xylose, mannose, and galactose) can be extracted from milled MH and LP through pressurized dilute acid treatment in maximum yields of 12.6 g/L and 15.3 g/L, respectively, representing 60.5% and 70.4% of the maximum possible yields, respectively. The crystallinity index increased upon pretreatment, reflecting the removal of the amorphous portion of biomass. The crystalline structure of the cellulose in the biomass, however, was not changed by the ASE extraction process.

초임계추출법을 이용한 브롬계 난연제 화합물 환경성 평가 추출효율 분석 연구 (Quantitative Extraction Analysis of Brominated Flame Retardant Substances Using Supercritical-Fluid Method for Environmental Assessment)

  • 오민경;윤상화;이영관;한재성;원성호;남재도
    • 폴리머
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    • 제32권1호
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    • pp.13-18
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    • 2008
  • 전기 전자재료 중 고분자에 포함된 브롬계 난연제의 분석에 있어 용출이 어려운 4가지 재질 PC(polycar-bonate) PP(polypropylene), PET(poly(ethylene terephthalate)), PBT(poly(butylene terephthalate))에 대하여 추출방법 및 헥산/에세톤, THF, 톨루엔, THF/톨루엔에 대한 용매 특이성과 그 특성을 고찰하였다. 각 고분자에서의 deca-BDE(decabromo diphenyl ether)의 함량을 속슬렛, 초음파. 가속용매, 마이크로파, 초임계 유체 추출법을 사용하여 이들 방법의 효율을 정량분석 하였다. 초음파 추출은 낮은 고분자의 용해도 때문에 낮은 추출효율을 보여 사용한 고분자의 경우에 있어서 추출방법으로는 적합하지 않았으며, 나머지 3가지 방법에서는 톨루엔 사용시 약 80% 이상의 높은 추출효율을 보였다. 초임계 유체 추출은 고분자의 난연제 추출에 시도되지 않았던 방법이었으나, 본 실험에서 PP와 PC의 추출에서는 100%에 가까운 매우 높은 추출효율을 보였다.

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.