• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.465-474
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• 1986

The solvent extraction and cleanup processes for the simultaneous gas-liquid chromatographic determination of 11 kinds of organophosphorous pesticide residues in crops were investigated. The extracts dissolved with acetone were partitioned with petroleum ether after adding saturated NaCl solution. Evaporated the partitioning solvent, the residue was dissolved in methylene chloride and eluted through mixed adsorbent (1 : 2 : 4 of activated carbon, magnesia and diatomaceous earth) with methylene chloride as an eluent. The pesticides recovered were 82∼105% and the impurities were effectively removed.

• Bulletin of the Korean Chemical Society
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• v.34 no.11
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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.

• Applied Chemistry for Engineering
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• v.18 no.2
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• pp.168-172
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• 2007

The separation of indole from a model mixture comprising four kinds of nitrogen heterocyclic compounds [indole (In), quinoline (Q), iso-quinoline (iQ), quinaldine (Qu)], three kinds of bicyclic aromatic compounds [1-methylnaphthalene (1MN), 2-methylnaphthalene (2MN), dimethylnaphthalene (DMN)], biphenyl (Bp) and phenyl ether (Pe) was examined by batch cocurrent 4 stages equilibrium extraction. The model mixture used as a raw material in this work was prepared according to the components and compositions contained in coal tar fraction (the temperature ranges of fraction: $240{\sim}265^{\circ}C$). An aqueous solution of formamide was used as a solvent. Indole was recovered more than 99% through 4 stages of the equilibrium extraction. The range of selectivity of indole in reference to DMN obtained through the 5 stages equilibrium extraction was found to be 63~118. The process for separation and recovery of indole contained in coal tar was studied by using the experimental results obtained from this work and the previous work.

• Journal of the Korean Chemical Society
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• v.33 no.1
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• pp.46-54
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• 1989

The extraction method and quantitative analysis for the fat-soluble vitamins present in food stuffs and vitamin products have been investigated. The simultaneous separation and analysis of the vitamins by reverse phase high performance liquid chromatographic method was conducted using an isocratic elution with methanol : water (95 : 5) eluent on a Novapak $C_{18}$ column. The detection of vitamins was achieved by a variable wavelength UV detector. To improve the detection sensitivity detection wavelengths were set at the highest absorption bands such as 330, 265, 285, and 290nm for the respective vitamins. The analysis for the fat-soluble vitamins was finished within 40 minutes. Alkaline hydrolysis and enzymatic hydrolysis were investigated for the sample preparation; and liquid-liquid extraction and liquid-solid extraction were attempted for the extraction of vitamins. Both hydrolysis methods were turned out to be appropriate for the analysis for vitamins A, D, and E, while for the analysis of vitamin K the enzymatic hydrolysis method demonstrated better results. Diethyl ether, pentane, and n-hexane were found to give higher recovery for the liquid-liquid extraction and silica cartridge for the liquid-solid extraction.

• Polymer(Korea)
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• v.32 no.1
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• pp.13-18
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• 2008

For the evaluation of brominated flame retardants included in polymeric electronic devices, we investigated the extraction methods and solvent systems for four different types of polymers of PC (polycarbonate), PP (polyropylene), PET (poly(ethylene terephthalate)) and PBT (poly(butylene terephthalate)) using different solvent systems of hexane/acetone, THF, toluene, and THF/toluene. In order to compare the extraction efficiency of different methods and solvent systems, the deca-BDE (decabromo diphenyl ether) flame retardant was included in PC, PP, PET and PBT systems and subsequently extracted by soxhlet, ultrasonic, accelerated solvent, microwave and supercritical fluid extraction methods. The amount of the extracted flame retardant was monitored to evaluate the extraction efficiency. The ultrasonic extraction method was found not to be acceptable as an extraction method for the polymer systems mainly due to a low salvation efficiency of the organic solvents. Soxhlet, accelerated solvent and microwave extraction methods exhibited over 80% of extraction efficiency for toluene. The supercritical fluid extraction method, which has been used as an extraction method for flame retardants in polymers, showed the extraction efficiencies of ca. 100% for PC and PP in the optimal extraction conditions of $60^{\circ}C$ and 120 bar.

• Bulletin of the Korean Chemical Society
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• v.25 no.10
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• pp.1465-1470
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• 2004

A short and efficient synthesis, solvent extraction and potentiometric measurements of new thiazole-containing naphtho-crown ethers are reported. The naphthalene moiety enhances the ammonium ion selectivity over potassium ion. The selectivity of ${NH_4}^+/K^+$ follows the trend $3\;{\approx}\;2\;>\;1$, indicating that the differences in conformational changes of 2 and 3 in forming ammonium complexes affect little on the resulting ammonium/potassium extraction selectivity ratio. The ammonium ion-selective electrodes were prepared with noctylphenyl ether plasticized poly(vinyl chloride) membranes containing 1-4 the effect of one naphthalene unit introduced on either right (2) or left (3) side of thiazolo-crown ether on their potentiometric properties (e.g., ammonium ion selectivity over other cations, response slopes, and detection limits) were not apparent. However, the ammonium ion selectivity of 1, 2 and 3 over other alkali metal and alkaline earth metal cations is 10-100 times higher than that of nonactin.

• Applied Biological Chemistry
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• v.40 no.5
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• pp.442-446
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• 1997

A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.

• Journal of Korean Society for Atmospheric Environment
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• v.16 no.6
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• pp.595-606
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• 2000

In order to compare analytical conditions for measuring PAHs(polycyclic aromatic hydrocarbons) in ambient air, a series of experiment were conducted using three different types of extraction methods that include:(1) accelerated solvent extraction (ASE), (2) soxhlet, and (3) sonification methods. Efficiency and relevant analytixal parameters for each of these methods were examined on five different types of solvents that include:(1) 10% diethyl ether in n-hexane(v/v), (2) dichloromethane, (3)cyclohexane.(4) toluene, and (5) Benzene: ethanol (4:1). Comparison of extraction efficiency for various combinations between methods and solvents was made through an application of both internal and external standard calibration techniques. The extraction efficiency tests, when checked using both internal and external standards, allowed us to derive meaningful comparison among different techniques and among solvents.

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.35-42
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• 2009

Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

• Journal of Ginseng Research
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• v.1 no.1
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• pp.29-32
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• 1976

Succinate dehydrogenase was activated by ethyl acetate extract from the methanol extract of white ginseng previously treated with petroleum ether and ethyl ether to remove all highly nonpolar components, and the residual aqueous solution from the ethyl acetate extraction. Also, all of the extracted fractions of red ginseng except the ether extract gave positive results. On the contrary to some suggestions by other workers that alkaloids of ginseng may enhance the succinate degydrogenase activity, our results show that the alkaloids may have exhibited some inhibitory eject on this enzyme.