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

• Bulletin of the Korean Chemical Society
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• 제35권2호
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• pp.371-376
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• 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
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• 제58권6호
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• pp.535-542
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• 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.