• 제목/요약/키워드: solid-phase extraction (SPE)

검색결과 200건 처리시간 0.025초

HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구 (Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC)

  • 오보영;배준현;강준길;김연두
    • 대한화학회지
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    • 제43권6호
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    • pp.663-669
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    • 1999
  • HPLC/UV 및 GC/FPD 법을 사용하여 환경수에 존재하는 Diazinon, EPN, Fenitrothion, Phosalon 및 Phosmet 등 5종의 유기인계 잔류농약을 분석하였다. 전처리 과정으로 고체상추출법(SPE)과 용매추출법(LLE)을 각각 적용한 결과, 회수율과 재현성에 있어, HPLC/UV에서는 용매추출법(LLE)보다 고체상추출법(SPE)이 더 우수하였고, GC/FPD에서는 고체상추출법(SPE)보다 용매추출법(LLE)이 더 우수하였다. 또 수돗물 및 하천수(와룡천)에 일정량의 유기인계 농약을 가하여 만든 합성시료중 각 성분을 분석한 결과, SPE-HPLC/UV 법에서는 회수율이 101%, % RSD는 4.3∼8.7이었고, LLE-GC/FPD 법에서는 회수율이 100%, % RSD는 3.2∼9.5이었다. 이 결과는 두 방법 모두 유기인계 잔류농약 분석에 이용할 수 있는 우수한 방법임을 제시하고 있다.

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The High-throughput Solid-Phase Extraction in the Field of Synthetic Biology: Applications for the Food Industry and Food Managements

  • Hyeri SEONG;Min-Kyu KWAK
    • 식품보건융합연구
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    • 제10권3호
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    • pp.19-22
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    • 2024
  • The field of synthetic biology has emerged in response to the ongoing progress in the life sciences. Advances have been made in medicine, farming, eating, making materials, and more. Synthetic biology is the exploration of using living organisms to create new organisms. By manipulating specific genes to express targeted proteins, proteins can be created that are both productive and cost-effective. Solid-phase extraction (SPE) and liquid-liquid extraction (LLE) are employed for protein separation during the production process involving microorganisms. This study centers on Scanning Probe Microscopy (SPM) to showcase its utility in the food industry and food management. SPE is predominantly utilized as a pretreatment method to eliminate impurities from samples. In comparison to LLE, this method presents benefits such as decreased time and labor requirements, streamlined solvent extraction, automation capabilities, and compatibility with various other analytical instruments. Anion exchange chromatography (AEC) utilizes a similar methodology. Pharmaceutical companies utilize these technologies to improve the purity of biopharmaceuticals, thereby guaranteeing their quality. Used in the food and beverage industry to test chemical properties of raw materials and finished products. This exemplifies the potential of these technologies to enhance industrial development and broaden the scope of applications in synthetic biology.

액체 추출법과 고체상 추출법에 의한 수질 중 유해물질 농축법 비교 (Comparison of Liquid-Liquid Extraction and Solid-Phase Extraction Coupled with GC/MS for Determination of Priority Pollutants in Water)

  • 육근성;홍사문;김종호
    • 분석과학
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    • 제7권4호
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    • pp.441-453
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    • 1994
  • 수질에서 유해물질을 농축하는 방법으로 액체 추출법과 고체상 추출법을 GC/MS를 검출기로 사용하여 비교하였다. 비휘발성 유해물질 중 11종의 산과 44종의 염기/중성 화합물들을 reagent water에 첨가하여 분석한 결과, 액체추출법은 54종의 화합물에 대해 91%의 평균회수율과 4.6%의 평균상대표준편차를 나타내었으며, 고체상 추출법은 52종의 화합물에 대해 63%의 평균회수율과 8.9%의 평균상대표준편차를 보였다. 두 방법의 검출한계는 $1{\sim}5{\mu}g/l$였다.

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디스크타입 고상추출장치 및 컬럼커플링을 이용한 물시료의 PCDD/Fs 간이분석법 (Fast Analytical Method of PCDD/Fs in Water by Combination of Disk Type Solid Phase Extraction and Column Coupling Chromatography)

  • 최재원;문부식;김경심;김정희;김순흥;백경희
    • 한국물환경학회지
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    • 제22권5호
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    • pp.879-886
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    • 2006
  • The analytical methods of polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans (PCDD/Fs) for water sample with extremely low concentration was developed to extract large volume and to improve fast chromatography for clean up. Semi-automated solid phase extraction (SPE) system and column coupling chromatography using elution pump was optimized and applied to each processes of treatment plant. Results of disk type SPE indicated that this system was applicable below 40 L of aqueous sample with a flow rate of 0.08 ~ 0.2 L/min. Average recoveries of SPE using labeled sampling spike of $^{37}Cl$-2,3,7,8-TCDD was 97%. Column coupling method resulted in reduced clean up time, solvent volume, increased average recoveries with constant elution rate. The combined methods were applied to the monitoring of drinking water treatment plant. Limits of detection (LOD) of each process were calculated. For example, LOD of raw and treated water ranged 0.094~0.968 pg/L and 0.028~0.364 pg/L, respectively. Combined methods of extraction and cleanup techniques provided fast analysis of PCDD/Fs with high accuracy and low LODs for water samples.

Solid-Phase Extraction of Caffeine and Catechin Compounds from Green Tea by Caffeine Molecular Imprinted Polymer

  • Jin, Yinzhe;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • 제28권2호
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    • pp.276-280
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    • 2007
  • In this work, caffeine and some catechin compounds + C, EC, EGC, and EGCG were extracted from green tea by using molecular imprinted polymers (MIP) as sorbent materials in a solid-phase extraction (SPE) process known as MISPE (molecular imprinted solid-phase extraction). For synthesis of MIP, caffeine was employed as the template, MAA as the monomer, EGDMA as the crosslinker, and AIBN as the initiator. A solution of caffeine (0.2 mg/mL in methanol) was utilized in the solid extraction cartridges following loading, washing, and elution procedures with acetonitrile, methanol, and methanol-acetic acid (90/10, %v/v) as the solvents, respectively. This solid-phase extraction protocol was applied for the extraction of caffeine and some catechin compounds from green tea. A comparison was made between the results obtained with the MIP cartridges and a traditional C18 reversed-phase cartridge. It was thereupon found that the recovery of caffeine by the MIPbased sorbent used in this work was almost two and four times greater than that by a commercially available C18 material. A quantitative analysis was conducted by high performance liquid chromatography (HPLC) using a C18 column (5 μm, 250 × 4.6 mm) with methanol/water (40/60, %v/v) as the mobile phase at a flow rate of 0.5 mL/min.

Comparison of Extraction Procedures for the Determination of Capsaicinoids in Peppers

  • Jeon, Geonuk;Lee, Jun-Soo
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1515-1518
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    • 2009
  • The objective of this study was to compare 3 extraction methods including, solid phase extraction (SPE), acetonitrile extraction, and methanol extraction, for their usefulness as extraction methods to determine capsaicinoids. The determination of capsaicinoids in the extracts was carried out on a reverse-phased high performance liquid chromatography (HPLC) using a fluorescence detector. Three extraction methods, i.e., SPE, acetonitrile extraction, and methanol extraction were compared for the quantification of capsaicinoids using raw peppers and pepper powder. The highest analytical values were observed using methanol extraction and the lowest values using SPE. Also, the analytical method validation parameters such as accuracy, precision, limit of detection, limit of quantitation, and specificity were calculated to ensure the method's validity. This method provides a fast and accurate approach for the determination of capsaicinoids in peppers.

콩나물중 benzimidazole계 농약의 추출방법과 잔류성 (An extraction method and residues of benzimidazole fungicides in soybean sprouts)

  • 박준조;용금찬;정진아
    • 농약과학회지
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    • 제4권1호
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    • pp.26-31
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    • 2000
  • 콩나물중 잔류농약의 효율적인 분석법을 확립하기 위하여 carbendazim과 thiabendazole을 0.1, 0.3, 0.5 mg/kg 씩 첨가하여 농약성분의 추출방법을 비교하였고, 잔류성을 평가하기 위하여 thiophanate-methyl 1.0, 2.0 g/L 용액에 수침시킨 콩으로 콩나물을 재배하면서 매일 잔류량을 조사하였으며, 또한 시중에 유통되는 콩나물중 benzimidazole계 농약의 잔류실태 조사를 실시하였다. 추출방법에 따라 carbendazim의 회수율은 LLE $69.25{\sim}79.16%$, SPE $79.99{\sim}90.42%$, MSPD $92.40{\sim}98.48%$이었으며, thiabendazole의 회수율은 LLE $64.86{\sim}83.26%$, SPE $79.12{\sim}94.04%$, MSPD $65.44{\sim}73.92%$로 고체상 추출방법이 우수하였다. 또 재배기간별 carbendazim 잔류량은 콩나물 출하적기인 재배 5일 째 $0.10{\sim}0.25$ mg/kg이었으며, 출하적기를 넘긴 7일째에도 농약이 잔류되었다. 유통 콩나물 448건을 검사한 결과 6건에서 carbendazim이 검출되었고 검출량은 3건에서 0.1 mg/kg 미만이었으나 3건에서는 0.1 mg/kg을 초과하여 최대 0.37 mg/kg까지 검출되었다.

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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.

울산지역 폐수 중 프탈레이트 에스테르 및 비스페놀 A(환경호르몬)의 GC/MS 분석

  • 한영주;박진도;이학성
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 2008년도 추계학술발표회 발표논문집
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    • pp.248-251
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    • 2008
  • 일반적으로 phthalate esters의 전처리방법에는 액액추출법(liquid-liquid extraction), 고상추출법(Solid-phase Extraction, SPE), 고상미세추출법(Solid-phase micro extraction, SPME) 등의 분석방법이 있다. 그 중에서 본 연구에서는 SPE를 이용하여 간편하고 정확성이 높으며, 적은 양의 유기용제를 사용하여 전처리함으로써 2차적인 환경오염을 줄일 수 있다는 점에서 다른 전처리 방법보다 유용하다고 할 수 있다. 검출감도 측면에서 phthalate esters의 경우는 구조적으로 안정적인 편이나 페놀류의 경우 hydroxy group 때문에 GC/MS 분석시 유도체화 과정이 필수적인데 이번 연구에서 사용한 BSTFA/TMCS는 비교적 쉽고 빠르게 유도체 화할 수 있다는 이점이 있다. 더 많은 연구가 필요하겠지만 앞서서의 결과에서도 알 수 있듯이 전반적으로 검출한계가 0.05$\sim$0.5 $\mu$g/L 정도로 높고, 4-nonyl phenol을 제외하고 80% 이상의 양호한 회수율을 나타낸 것으로 미루어 보아 phthalate esters, phenols의 효율적인 동시분석이 가능함을 알 수 있다.

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울산지역 폐수 중 프탈레이트 에스테르 및 비스페놀 A의 HPLC 분석

  • 한영주;박진도;이학성
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 2008년도 추계학술발표회 발표논문집
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    • pp.272-274
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    • 2008
  • 일반적으로 프탈레이트 에스테르의 전처리방법에는 액액추출법(Liquid Liquid Extraction, LLE), 고상추출법(Solid Phase Extraction, SPE), 고상미세추출법(Solid Phase Micro Extraction, SPME) 등의 분석방법이 있다. 그 중에서 본 연구에서는 간편하고 정확성이 높은 SPE를 이용하였으며, 적은 양의 유기용제를 사용하여 전처리함으로써 2차적인 환경 오염을 줄일 수 있다는 점에서 다른 전처리 방법보다 유용하다고 할 수 있다. 또한 프탈레이트 에스테르의 경우는 구조적으로 안정적인 편이나 페놀류의 경우 hydroxy group 때문에 GC/MS 분석시 유도체화 과정이 필수적이나 이번 연구에서는 HPLC를 이용하므로 별도의 유도체화의 번거로움 없이 바로 분석할 수 있는 이점이 있다. 더 많은 연구가 필요하겠지만 앞서서의 결과에서도 알 수 있듯이 전반적으로 검출한계가 0.1$\sim$0.5$\mu$g/L 정도로 높고, 82% 이상의 양호한 회수율을 나타낸 것으로 미루어 보아 극미량 분석이 아닌 이상, 산업체에서 HPLC의 이용이 더욱 유리할 것이라고 사료된다.

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