• 한국기계가공학회지
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• 제19권10호
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• pp.1-7
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• 2020

In this study, a multichannel gas-liquid microextraction system is designed by integrating the automatic elution of extraction line and multichannel gas-purging liquid phase microextraction. The system uses an injection pump and inert gas to push the extraction solvent to a sample bottle of a gas-phase color autosampler and then implements multichannel gas-liquid microextraction and gas chromatography-mass spectrometry. The system also employs a three-way integrated micro-high-temperature heater, syringe pump, and microflow controller to realize the simultaneous processing of multiple groups of samples, thus improving the sample pretreatment speed and reproducibility and reducing human error. Autoinjection experiments were implemented with polycyclic aromatic hydrocarbon standard samples. The experiments show that the average recovery rate of the system exceeds 70%, and the relative standard among the channels is less than 15%.

• 공업화학
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• 제26권1호
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• pp.17-22
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• 2015

2013년 시리아 내전 간 사용되어 1,300명 이상의 사망자를 발생시킨 사린(GB) 등의 화학무기로 인해 화학무기에 대한 국제적 관심이 다시 한번 높아지게 되었다. 화학작용제는 자연환경에 노출이 되면 가수분해(hydrolysis) 또는 광분해(photodegradation) 과정을 거쳐 분해물질로 분해된다. 화학작용제 및 분해물질(가수분해 또는 산화된 생성물)은 통상수 ppb 정도의 낮은 농도로 존재하기 때문에 정확한 샘플분석을 위해서는 화학작용제 및 분해물질을 환경샘플로부터 분리, 추출, 농축시키는 전처리 과정이 필요하다. 용매추출법(LLE), 고체상 추출법(SPE) 등이 화학작용제의 전처리 방법으로 많이 사용되나 최근에는 사용되는 용매의 양은 줄이면서 분석효율은 높일 수 있는 liquid phase microextraction (LPME)이 개발 적용되고 있다. 본 리뷰에서는 화학작용제 및 그 분해물질의 전처리에 활용된 LPME 전처리 기법에 대해 살펴보고자 한다.

• 분석과학
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• 제18권3호
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• pp.224-231
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• 2005

잔류농약 분석에 전통적으로 사용되는 액체-액체 추출법과 액체-고체 추출법의 여러 가지 단점을 극복하고 기존의 낮은 정밀도와 저조한 추출효과를 보완하기위해 자동화된 장치를 이용한 액체상 극미량 추출법(Liquid Phase Microextraction : LPME)을 사용하였으며 이에 대한 최적화 조건을 설정하였다. 대상농약은 demeton-S-methyl, diazinon, parathion, fenitrothion, EPN등 5종이었으며 채소 시료 중에서 추출하여 HP 6890 GC/NPD를 사용하여 분석하였다. 자동화된 LPME를 이용한 최적의 추출조건은 pH 3, 염의 농도 $100{\mu}g/mL$이었으며 검량선을 작성하였을 때 $0.2{\sim}10{\mu}g/g$ 범위에서 $R^2=0.9921$ 이상 직선상의 상관관계를 나타내었고 $5{\mu}g/g$ 농도에서 demeton-S-methyl은 7.7%, diazinon은 9.8%, parathion은 7.8%, fenitrothion는 9.7%, EPN은 8.2%의 상대표준편차를 나타내었고 정확도는 demeton-S-methyl는 12.7%, diazinon는 7.8%, parathion는 10.4%, fenitrothion는 -6.7%, EPN은 -0.7%로 좋은 값을 나타내었다.

• Bulletin of the Korean Chemical Society
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• 제27권2호
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• pp.231-236
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• 2006

A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

• 분석과학
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• 제30권4호
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• pp.174-181
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• 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
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• 제26권12호
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• pp.1996-2000
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• 2005

Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

• 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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• 제35권4호
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• pp.1011-1015
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• 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.

• 대한화학회지
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• 제54권1호
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• pp.38-42
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• 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.

• 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.