• Bulletin of the Korean Chemical Society
• /
• 제34권11호
• /
• pp.3444-3450
• /
• 2013

Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

• 대한화학회지
• /
• 제54권1호
• /
• pp.38-42
• /
• 2010

인간뇨의 마트린 알칼로이드의 결정을 위한 민감한 정량적 방법은 HPLC에 결합된 중공섬유 액상 미세추출을 기반으로 개발되었다. pH를 포함하여 HF-LPME 효율의 다양한 인자의 영향과 공급 용액의 이온세기, 수용체용액의 pH, 교반율 그리고 추출시간이 조사되었다. 최상의 HF-LPME 조건은 다음과 같다: 1-octanol이 중공섬유의 기공안에 주입된다, 중공섬유의 루멘에 pH 1.50의 100 mmol/L of $H_3PO_4$ 수용체 용액을 주입한다, 1 mol/L NaOH는 공급 용액의 pH, 600 rpm의 교반속도와 60분의 추출시간을 조정하여 사용된다. LPME의 방법은 실제의 소변 샘플에서 마트린과 소포카르핌의 분석에 성공적으로 적용되었다.

• 분석과학
• /
• 제30권4호
• /
• pp.174-181
• /
• 2017

Bio-liquid is a liquid by-product of the hydrothermal carbonization (HTC) reaction, converting wet biomass into solid hydrochar, bio-liquid, and bio-gas. Since bio-liquid contains various compounds, it requires efficient sampling method to extract the target compounds from bio-liquid. In this research, fatty acid methyl ester (FAME) in bio-liquid was extracted based on hollow fiber supported liquid phase microextraction (HF-LPME) and determined by Gas Chromatography-Flame Ionization Detector (GC-FID) and Gas Chromatography/Mass Spectrometry (GC/MS). The well-known major components of biodiesel, including methyl myristate, palmitate, methyl palmitoleate, methyl stearate, methyl oleate, and methyl linoleate had been selected as standard materials for FAME analysis using HF-LPME. Physicochemical properties of bio-liquid was measured that the acidity was 3.30 (${\pm}0.01$) and the moisture content was 100.84 (${\pm}3.02$)%. The optimization of HF-LPME method had been investigated by varying the experimental parameters such as extraction solvent, extraction time, stirring speed, and the length of HF at the fixed concentration of NaCl salt. As a result, optimal conditions of HF-LPME for FAMEs were; n-octanol for extraction solvent, 30 min for extraction time, 1200 rpm for stirring speed, 20 mm for the HF length, and 0.5 w/v% for the concentration of NaCl. Validation of HF-LPME was performed with limit of detection (LOD), limit of quantitation (LOQ), dynamic range, reproducibility, and recovery. The results obtained from this study indicated that HF-LPME was suitable for the preconcentration method and the quantitative analysis to characterize FAMEs in bio-liquid generated from food waste via HTC reaction.

• Bulletin of the Korean Chemical Society
• /
• 제35권4호
• /
• pp.1011-1015
• /
• 2014

Octadecyl-modified graphene (graphene-C18) was fabricated and used as adsorbent in hollow fiber liquid phase microextraction (HF-LPME) for the first time. The extraction performance of graphene-C18 reinforced HF-LPME was evaluated using chlorophenols as model analytes. The factors affecting the extraction efficiency, such as extraction time, pH of the sample solution, agitation rate, the concentration of graphene-C18 and salt addition were optimized. After the graphene-C18 reinforced HF-LPME of the chlorophenols from honey sample, the analytes were separated and determined by high-performance liquid chromatography. The linearity was observed in the range of 5.0-200.0 ng $g^{-1}$ for 2-chlorophenol and 3-chlorophenol, and 2.0-200.0 ng $g^{-1}$ for 2,3-dichlorophenol and 3,4-dichlorophenol, respectively. The limits of detection (S/N = 3) of the method were lower than 1.5 ng $g^{-1}$. The recoveries of the method were between 88% and 108%. The method is simple, sensitive and has been resoundingly applied to analysis of chlorophenols in honey samples.

• 분석과학
• /
• 제21권2호
• /
• pp.84-92
• /
• 2008

속빈 섬유-액상 미량추출법(hollow fiber-liquid phase microextraction, HF-LPME)과 기체 크로마토그래프/질소-인 검출기(GC-NPD)를 사용하여 사람의 뇨와 여러 가지 음료 중에서 극미량의 카페인을 분석하는 방법을 확립하였다. 수용액 시료로부터 카페인의 양을 측정하기 위해서 속빈 섬유의 길이, 추출용매의 종류, 교반효과, pH 및 염석효과 등 여러 가지 실험적인 파라미터를 변화시켜서 최적의 조건을 확립하고자 하였다. 검정곡선의 회귀계수($r^2$)는 0.9994이상이었으며, 평균 상대 회수율은 102%(n=3)이었으며, 기기검출한계는 2.5 ng/mL, 정량한계는 10 ng/mL이었다. 확립된 HF-LPME 방법은 생물학적 시료, 음식물, 환경시료 중에서 카페인의 농도를 측정하기에 편리하고 정확한 방법이 될 것이다.

• Bulletin of the Korean Chemical Society
• /
• 제35권2호
• /
• pp.371-376
• /
• 2014

A novel three-phase hollow fiber liquid phase microextraction was developed for the determination of malachite green (MG) in environmental waters, which selected [BMIM][$PF_6$] mixed with 1% trioctylphosphine oxide (TOPO) as supported phase. Several parameters (accepter phase pH, sample pH, supported phase membrane, volume of accepter phase, salinity, extraction time) that could affect extraction performance were investigated. Under the optimal extraction conditions, the established approach showed excellent characters as: high enrichment factor (212), wide linear range ($0.20-100{\mu}gL^{-1}$), low detection limit ($0.01{\mu}gL^{-1}$), good reproducibility (RSD, 8.9%, n=5) and satisfactory recovery (84.0-106.2%). The method was applied to detect MG at Yangtze River and pond waters in Zhenjiang, Jiangsu province, and 4 sites among 15 sampling sites were found MG with the concentration of $1.73-11.06{\mu}gL^{-1}$, which confirmed that the proposed environmentally friendly method was simple and effective for monitoring MG in aquatic system.

• 대한화학회지
• /
• 제58권6호
• /
• pp.535-542
• /
• 2014

간편하고 효율적이며 친환경적인 시료전처리 방법인 3-상 속빈 섬유 액체상 미량추출법(3-phase HF-LPME) 및 HPLC-UV/Vis를 이용하여 소변 중에 존재하는 테트라사이클린류 항생제 3종(tetracycline, oxytetracycline, chlortetracycline)을 동시에 분석하는 방법을 개발하였다. 분석 물질은 $C_8$ 컬럼($150{\times}3.0mm$, $3{\mu}m$)을 사용하여 기울기 용리법으로 분리되었으며 높은 선택성과 감도를 나타내었다. 시료 전처리를 위한 최적의 실험조건을 확립하였는데, 추출용매로는 heptanal, 추출시간은 60분, 주개 상의 pH는 9.0, 받개 상의 pH는 1.0, 시료의 교반속도는 700 rpm, 추출 시간은 60분이었으며 농축인자는 5.6~22.3이었다. 검출한계와 정량한계는 각각 $0.08{\sim}0.8{\mu}g/mL$와 $0.4{\sim}1.6{\mu}g/mL$이었으며, $0.1{\sim}32{\mu}g/mL$ 농도범위의 검정곡선은 좋은 직선성($R^2$ >0.995)과 정밀도(1.3~9.1 RSD %) 및 정확도(84~118%)를 나타냈다.