• 제목/요약/키워드: Two-phase extraction

검색결과 272건 처리시간 0.025초

일단계 추출 및 메칠화법에 의한 유료작물의 지방산 분석 (Fatty Acid Composition Analysis of Major Oil Crops by One-Step Extraction/Methylation Method)

  • 김진경;김남희;방진기;이병규;박충범;이봉호
    • 한국작물학회지
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    • 제45권3호
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    • pp.211-215
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    • 2000
  • 시료의 지방산 분석은 먼저 지방의 추출이 선행되어야 하는데 이때에는 시료량 및 시약이 많이 들고 또한 분석시간이 많이 소요되므로 지방 추출 및 지방산의 에스테르화를 한 단계에서 실시하는 One step extraction/methylation법(방법 1)에 따라 주요 유료작물의 지방산 조성을 살펴보았다 이 방법은 methanol-heptane-benzene-DMP-H$_2$SO$_4$ 혼합용매를 사용하여 지방 추출 및 지방산 에스테르화를 단일층에서 일어나게 한것으로 기존의 sodium methoxide를 촉매로 한 methanolysis 법에 의한 지방산 분석 결과와 유의적인 차이를 보이지 않았다. 또한 이 혼합시약으로 이미 추출된 지방을 대상으로 실험하였을 때에도(방법 2) 기존방법과 유의적인 차이가 없었다. 따라서 이 One step extraction/methylation법은 시료가 생체이든 추출된 지방이든 그 과정이 단순하고 시간과 노력이 훨씬 적게 소요되어 지방산 분석에 널리 이용될 수 있을 것이며, 특히 1회에 많은 시료를 처리하고자 할 때 더욱 분석효율이 높을 것으로 기대되었다

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고체상 추출과 GC/MS를 이용한 소변 중 대마 대사체 (THCCOOH) 분석 (Determination of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) in human urine by solid-phase extraction and GC/MS)

  • 정재철;김진영;인문교;정원조
    • 분석과학
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    • 제19권5호
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    • pp.441-448
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    • 2006
  • 소변 중 대마 남용여부를 판별하는데 기준이 되는 tetrahydrocannabinol (THC)의 대사체 성분인 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH)를 고체상 추출법 (solid-phase extraction, SPE)과 가스크로마토그래피/질량분석법 (GC/MS)을 이용하여 신속하게 분석 할 수 있는 방법을 제시하였다. 본 실험은 시험관에 소변 3 mL를 취해 염기성 (pH 10) 조건에서 가수분해 한 후, 양이온교환 카트리지를 사용하여 THCCOOH 성분을 선택적으로 추출하고, 증발 건고한 다음 유도체 반응을 시켜 GC/MS로 분석하였다. 그 결과 분석방법의 검출한계 (LOD)는 0.4 ng/mL이고, 정량한계 (LOQ)는 1.2 ng/mL이였다. 검정곡선의 직선성 상관계수 ($r^2$)는 1.2 (LLE는 1.3)~50.0 ng/mL의 농도범위에서 0.999를 나타내었다. 그리고 정밀도 (precision)와 정확도 (accuracy)는 모두 ${\pm}1.20%$ 이내로 안정적이었으며, 회수율(recovery)은 83.6~90.7%로 측정되었다. 액체상 추출법 (liquid-liquid extraction, LLE)과 비교할 때, SPE 방법이 회수율은 낮았지만 검출한계, 정량한계, 정밀도 및 정확도에서는 큰 차이가 없었다. 그러나 LLE 방법은 추출과정에 시간과 노력이 많이 드는 반면, SPE 방법은 상대적으로 추출 조작이 간편하고 신속하게 추출되었으며, 추출 잔류물도 깨끗하였다. SPE를 이용한 추출방법을 다수의 대마 흡연자 소변에 적용하였을 때 기존에 사용하던 LLE 방법보다 간편하고, 신속하게 대마 대사체 분석이 가능하였다.

Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

  • Lee, In Ja;Ahn, Jae-Chan;Kim, Bogsoon;Chung, Deukmo
    • Mass Spectrometry Letters
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    • 제8권1호
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    • pp.18-22
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    • 2017
  • Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

Valencia 오렌지로부터 내열성 Pectinesterase의 추출 (A Study on the Extraction of Thermostable Pectinesterase from Valencia Orange)

  • 허원녕
    • 한국식품과학회지
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    • 제27권5호
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    • pp.658-665
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    • 1995
  • Pectinestrase(PE) 중에 열에 안정한 thermostable pectineterase(TSPE)를 열에 불안정한 thermolabile pectinesterase(TLPE)로부터 구분하기 위하여 $70^{\circ}C$에서 $5{\sim}10$분간 가열 처리하였다. TSPE의 추출 수율을 증가시키기 위하여 추출시간, pH, 온도, NaCl의 농도 그리고 세포벽을 분해하는 가수분해 효소의 사용 등 여러가지 변화를 주어 개발한 최적 조건은 오렌지 착즙액의 pH 4.14와 같은 1 M NaCl의 acetate buffer에 분말시료의 0.2% $Cytolase^{TM}$ 104(cellulase hemicellulase와 pectinase의 혼합물) 첨가하여 가수분해하여 추출하는 것이었다. 증류수로 추출하거나 황산암모늄 $0{\sim}0.3$ 포화도의 분획은 목적으로 하는 PE 이외의 단백질을 제거하는 수단으로 이용할 수 있었다. 또한 5.0% Triton TX-114의 두가지 액상을 이용한 분배의 방법은 추출한 조효소로부터 TLPE와 TSPE를 분리하는 수단으로 이용할 수 있었다.

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Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • 제45권1호
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.

하수처리시설 고상시료 중 잔류의약물질 분석을 위한 전처리법 평가 및 적용 (Evaluation and application of pretreatment methods for pharmaceuticals and personal care products in the solid phase of sewage samples)

  • 박준원;김창수;주병규;이원석;정현미;정동환
    • 상하수도학회지
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    • 제32권6호
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    • pp.559-572
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    • 2018
  • The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

Removal of Pollutants and Recovery of Toxic Heavy Metals from Wastewater Using Microporous Hollow Fiber Modules

  • Yun, Chang-Han
    • 한국막학회:학술대회논문집
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    • 한국막학회 1993년도 춘계 총회 및 학술발표회
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    • pp.25-27
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    • 1993
  • Multiphase equilibrium-based processes for separation and purification generally utilize dispersed systems in which one phase is dispersed in the other as bubbles or drops or thin films. Using microporous membranes, novel techniques have been developed such that multiphase processes can now be carried out in a nondispersive fashion for gas-liquid (Sirkar, 1992) and liquid-liquid (Prasad and Sirkar, 1992) contacting processes. Among such processes, only nondispersive solvent extraction of pollutants using microporous membranes will be of concern here. These processes employ immobilized immiscible phase interfaces at the pore mouths in a microporous membrane. Through such interfaces, solutes are extracted into the solvent as two immiscible phases flow on two sides of a microporous membrane. Many advantages of such a technique over conventional dispersion-based extractors have been summarized (Prasad and Sirkar, 1992).

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Determination of Terbutaline Enantiomers in Human Plasma by Coupled Achiral-Chiral High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Kim, Hyun-Ju;Hong, Seon-Pyo;Shin, Sang-Deok
    • Archives of Pharmacal Research
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    • 제23권5호
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    • pp.441-445
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    • 2000
  • Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column, The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/$m\ell$ (r=0.9999) and detection limit was 1.0 ng/$m\ell$ .

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간소화된 윈도우 푸리에 위상을 이용한 계층적 접근기반의 3차원 객체 추출 기법 (3D Object Extraction Algorithm Based on Hierarchical Approach Using Reduced Windowed Fourier Phase)

  • 민각;한규필;이기수;하영호
    • 한국통신학회논문지
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    • 제27권8A호
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    • pp.779-785
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    • 2002
  • 본 논문에서는 두 개의 2차원 영상에서 3차원 객체를 효율적으로 추출하기 위해서 위상 기반의 스테레오 정합 알고리즘을 제시한다. 특히, 윈도우 푸리에 위상을 이용하는 기존의 위상 기반 방법들은 기본적으로 다중-해상도 위상 맵을 사용하기 때문에 계층적인 접근 관점에서 좋은 특성을 가지고 있는 반면 높은 계산량을 요구한다. 그러므로 본 논문에서는 다중-해상도 위상 기반전략과 더불어 위상 계산의 중복성을 제거하는 빠른 계층적 접근기반의 3차원 객체 추출 기법을 제안한다. 또한, 정합 성능을 개선시키기 위해 위상 영역에서 형태학적인 정합 알고리즘을 제시한다. 제안된 알고리즘을 실험한 결과 계산량이 대략 8배 정도로 크게 감소되었으며 안정된 결과 값을 획득할 수 있었다.

양송이 색소의 특성과 염색성에 관한 연구(I) - 색소의 추출과 보관 및 성분 분석을 중심으로 - (A Study on the Characterization and Dyeability of Mushroom Colorant (I)- Extraction, storage and analysis of mushroom colorant-)

  • 서영숙;정지윤
    • 한국의류학회지
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    • 제21권1호
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    • pp.228-236
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    • 1997
  • The browning characteristic and dyeability of the mushroom were examined to establish the optimum condition for browning and extraction in the process of obtaining the natural dye, brown colorant. The composition of browning extracts from mushroom was also analyzed and the dyeability were investigated. The results of this study are as follows, 1. The optimum condition for obtaining the browning colorant from mushroom was the crushed phase of sample. 2. The browning reaction by enzymes in mushroom was efficient at a temperature of 35$^{\circ}C$, a duratron period of 2 hr and pH of 8. 3. The optimum condition for extraction of browning extracts from browned mushroom was at 95$^{\circ}C$ and Ihr. 4. To analyze the content of browning extracts in the mushroom, three fractions were obtained from gel filtration using Sephadex G-25 and the fraction 1 was melanin and the fraction 3 was dihydroxyphenylanine (DOPA) and glutaminyldihydroxybenzene (GDHB) . 5. The turbidity in enzymatic browning extraction of mushroom increased depending on refrigeration storage (4$^{\circ}C$) and UV radiation. The filtration of the extracts resulted in a decrease of absorbance. 6. The dyeability of the fraction 1 was greater compared to that of the fraction 3 and that of wool greater compared to the other two fabric materiales.

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