• 분석과학
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• 제17권4호
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• pp.295-301
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• 2004

In this study, static and dynamic solvent extractions are compared for more efficient extraction of polychlorinated dibenzofurans (PCDFs) from fly ash. Static solvent extraction rather than dynamic extraction showed a higher recovery of PCDFs, which was adsorbed strongly with fly ash. The effects of parameters, such as temperature, toluene-isopropyl alcohol mixture, static and dynamic time flow rate, and solvent volume on the extraction were investigated and the variations in average recoveries of PCDFs were explained. In both extractions, temperature was an effective parameter because the higher temperature gave the higher recoveries. In dynamic solvent extraction, dynamic time was more effective than flow rate and solvent volume for the extraction of PCDFs from fly ash. Multi-layer column chromatography on neutral and acidic silica gel with n-hexane was used for cleaning up the extracts. The quantification of the PCDFs extracted was performed using HPLC-UV.

• KSBB Journal
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• 제29권2호
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• pp.98-105
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• 2014

Three different types of extraction processes, which used supercritical carbon dioxide ($SCCO_2$) and organic solvent, were attempted to improve the extraction yield of oil from Chlorella vulgaris: cosolvent-modified $SCCO_2$ extraction, $SCCO_2$ extraction with ultrasonic sample treatment in organic solvent, and static extraction with organic solvent followed by dynamic $SCCO_2$ extraction. Among these, the last $SCCO_2$ extraction process was found to be most effective in the extraction of oil. Compared with pure $SCCO_2$ extraction, the extraction yield of oil was observed to increase about 7 times.

• Bulletin of the Korean Chemical Society
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• 제20권6호
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• pp.689-695
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• 1999

Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins(PCDDs) from the XAD-2 resin which was used to adsorb PCDDs in the atmosphere. XAD-2 resin spiked with five PCDDs was chosen as a sample. The optimum conditions for the extraction of PCDDs by SFE were turned out to be the use of CO2 modified with 10% toluene at 100 ℃ and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDDs ranging from 68 to 98%. The ultrasonic extraction of PCDDs from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDDs for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of tem-perature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was n-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDDs ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations.

• 약학회지
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• 제36권6호
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• pp.563-569
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• 1992

The sorption and desorption properties of four different solid adsorbents were evaluated for the trace enrichment of ibuprofen from biological samples. Chromosorb 107 gave the highest dynamic adsorption coefficient. Among the organic solvents examined, acetone gave the highest desorption coefficient. Using the Chromosorb 107 column, the optimum elution volume of the eluting solvent was evaluated from the breakthrough curve of ibuprofen. The usefulness of Chromosorb 107 as the solid adsorbent and acetone as the eluting solvent was examined for the solid-phase extraction of ibuprofen from serum in the concentration range of $20{\sim}40\;{\mu}g/ml$.

• 약학회지
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• 제39권4호
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• pp.395-400
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• 1995

The sorption and desorption properties of four adsorbents were evaluated for the trace enrichment of clobazam from biological samples. Graphitized carbon black(GCB) gaved the highest dynamic adsorption coefficient. Among the six organic solvents examined, acetone gave the highest desorption coefficient for the clobazam adsorbed on GCB. Using the GCB column, the optimum elution volume of the eluting solvent was evaluated from the on-line monitored breakthrough curve for clobazam. When GCB as the solid adsorbent and acetone as the eluting solvent were used for the solidphase extraction of clobazam from serum, the recoveries were higher than 83% with good reproducibility in the concentration range of 20-50 $\mu\textrm{g}$/ml.

• Bulletin of the Korean Chemical Society
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• 제28권12호
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• pp.2389-2395
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• 2007

Headspace solid phase trapping solvent extraction (HS-SPTE) and GC-MS was applied for the characterization of volatile flavors from fennel, anise seed, star-anise, dill seed, fennel bean, and Ricard aperitif liquor. Tenax was used for HS-SPTE adsorption material. Recoveries, precision, linear dynamic ranges, and the limit of detection in the analytical method were validated. There were some similarities and distinct differences between fennel-like samples. The Korean and the Chinese fennels contained trans-anethole, (+)-limonene, anisealdehyde, methyl chavicol as major components. The volatile aroma components from star anise were characterised by rich trans-anethole, (+)-limonene, methyl chavicol, and anisaldehyde. Additionally, principal component analysis (PCA) has been used for characterizing or classifying eight different fennel-like samples according to origin or other features. A quite different pattern of dill seed was found due to the presence of apiol (dill).

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3603-3609
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• 2011

A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

• Bulletin of the Korean Chemical Society
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• 제27권5호
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• pp.649-656
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• 2006

The proposed head-space supercritical fluid extraction (SFE) methodology as an alternative to an existing conventional procedure was explored for the determination of organochlorine compounds in aqueous matrix. In this study, polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) were utilized as target analytes. To enhance the recovery efficiency, the factors such as the $CO _2$ density, the extraction time, and the extraction mode were investigated. Furthermore, the analytical procedures and the results obtained were compared with those provided by the conventional method (the U.S. EPA method 8080). Under the optimized conditions, i.e., a combination of static with dynamic SFE mode at 2,000 psi and 40 ${^{\circ}C}$, the head-space SFE methodology gave equivalent or better to the conventional method in recovery efficiencies with clear advantages such as simple sample treatment and fast analysis time as well as reduced solvent and reagent consumption.

• 분석과학
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• 제28권6호
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• pp.436-445
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• 2015

한약재 중 항산화 작용이 있다고 알려진 사인(Amomi Fructus)을 SDE (simultaneous distillation extraction) 방법으로 정유(essential oil)를 추출하고 GC-MS (gas chromatography-mass spectrometry)를 이용하여 39개의 성분을 규명하였으며, 주요 성분은 camphor, borneol acetate, borneol, D-limonene 및 camphene이었다. 유기용매 3가지(헥세인, 다이에틸 에터 및 다이클로로메테인)를 이용하여 얻은 용매 추출물에서 정유성분 이외에 추가로 4개의 성분을 규명하였으며, 주요 5개 성분은 동일하였으나 상대적인 면적 비율은 차이가 있었다. 특정온도와 휘발 조건에서 정유와 용매 추출물에서 휘발하는 물질들의 종류와 상대적인 비율을 측정하기 위하여 dynamic headspace를 이용하여 특정 조건에서 휘발하는 물질들을 트랩에 포집한 후 GC-MS로 분석하였다. 사인으로부터 SDE 방법에 의해 정유를 추출하는 방법의 회수율을 장뇌(camphor)를 이용하여 측정하였으며, 장뇌의 회수율은 82.0% 이었다. 사인에서 Hg의 함량은 수은 분석기로 측정하였으며, Cd, Pb, Cr, Mn, Co, Ni, Cu 와 Zn은 ICP-MS (Inductively coupled plasma-mass spectrometer)로 측정하였다. 사인에서 Pb, Cd 및 Hg이 각각 0.72 mg/kg, <0.10 mg/kg 및 0.0023 mg/kg 검출되었으며, 이는 순도시험 허용기준치 이하의 값들이었다. 사인에서 Cr, Mn, Co, Ni, Cu와 Zn의 함량을 조사한 결과 Mn (213 mg/kg), Cu (8.29 mg/kg) 및 Zn (31.0 mg/kg)등이 비교적 높은 함량으로 검출되었으며, 정유와 용매 추출물에서도 Mn (0.65~9.08 mg/kg), Cu (1.16~4.40 mg/kg) 및 Zn (1.10~3.80 mg/kg)이 검출되었다. 이들 금속성분이 사인에서 기인하는 것인지 아니면 유통과정이나 취급과정에서 오염된 것인지의 여부 규명이 필요하며, 또한 이런 금속들이 생물학적 활성 연구에 어떤 영향 주는지도 규명할 필요가 있다.

• Mass Spectrometry Letters
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• 제8권1호
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• pp.8-13
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• 2017

Analysis of quinidine for fish tissues using single drop microextraction (SDME) coupled with atmospheric pressure matrix assisted laser desorption/ionization mass spectrometry (AP-MALDI-MS) are reported. Optimization conditions; such as extraction solvent, extraction time, pH of the aqueous solution, salt additions (NaCl), stirring rate, matrix type and concentration are investigated. Linear dynamic range (${\mu}M$), limit of detection, relative recovery%, and enrichment factor are 0.08-9.2, 0.05, $94.8{\pm}3.1-98.5{\pm}3.3%$, $4.34{\pm}0.28-4.40{\pm}0.30$, respectively. SDME-AP-MALDI-MS shows good intraday and interday reproducibility.