• The Korean Journal of Food And Nutrition
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• v.21 no.2
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• pp.143-147
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• 2008

To develop a new anti-wrinkle agent from medicinal plants, this study investigated the optimal conditions for extracting elastase inhibitor from Rheum undulatum L. Maximal extraction occurred by using 70% methanol at $50^{\circ}C$ for 24 hr; the elastase inhibitory activity was 60.4%($IC_{50}:6.7{\times}10^3{\mu}g/m{\ell}$). Systematic solvent extraction, thin layer chromatography, silica gel column chromatography, Sephadex LH-20 column chromatography, and reverse-phase high performance liquid chromatography were used in the partial purification of the elastase inhibitor. The compound was soluble in dimethylsulfoxide, methanol, and ethanol, and had maximum absorption spectra at 231.5 nm and 275.5 nm.

• Journal of Microbiology and Biotechnology
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• v.25 no.5
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• pp.704-708
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• 2015

For the analysis of multiple-reaction intermediates for long-chain dicarboxylic acid biotransformation, simple and reproducible methods of extraction and derivatization were developed on the basis of gas chromatography with flame ionization detector (GC-FID) instead of mass spectrometry. In the derivatization step, change of the ratio of pyridine to MSTFA from 1:3 to 9:1 resulted in higher peak intensity (p = 0.021) and reproducibility (0.6%CV) when analyzing 32 g/l ricinoleic acid (RA). Extraction of RA and ω-hydroxyundec-9-enoic acid with water containing 100 mM Tween 80 showed 90.4-99.9% relative extraction efficiency and 2-7%CV compared with those with hydrophobic ethyl acetate. In conclusion, reduction of the pyridine content and change of the extraction solvent to water with Tween 80 provided compatible derivatization and extraction methods to GC-FID-based analysis of longchain carboxylic acids.

• Korean Chemical Engineering Research
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• v.60 no.4
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• pp.499-505
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• 2022

This study presents a conceptual design of vanillin production from Kraft lignin. Most of the existing Kraft lignin is used as low-quality boiler fuel or discarded as wastewater, and only 2% or less of lignin has been refined into high-quality products. We propose the process developed in this study to utilize discarded Kraft lignin. The existing vanillin production concept process consisted of alkali oxidation using NaOH, filtration, chromatography, and crystallization. Chromatography, which is difficult to commercialize, was changed to a solvent extraction process. The recovery rate of vanillin of the proposed solvent extraction process is 92.9%, and the purity is 99.5%, which is similar to the existing chromatography process. The reason why the solvent extraction process showing similar results to chromatography can replace the existing chromatography process was analyzed.

• Analytical Science and Technology
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• v.31 no.3
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• pp.112-121
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• 2018

The hydrothermal carbonization method has received great attention because of the conversion process from biomass. The reaction produces various products in hydrochar, bio-liquid, and gas. Even though its yield cannot be ignored in amount, it is difficult to find research papers on bio-liquid generated from the hydrothermal carbonization reaction of biomass. In particular, the heterogeneity of feedstock composition may make the characterization of bio-liquid different and difficult. In this study, bio-liquid from the hydrothermal carbonization reaction of food wastes at $230^{\circ}C$ for 4 h was investigated. Among various products, fatty acid methyl esters were analyzed using two different extraction methods: liquid-liquid extraction and column chromatography. Different elutions with various solvents enabled us to categorize the various components. The eluents and fractions obtained from two different extraction methods were analyzed by gas chromatography with a mass spectrometer (GC/MS). The composition of the bio-liquid in each fraction was characterized, and seven fatty acid methyl esters were identified using the library installed in GC/MS device.

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.61-66
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• 2009

An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

• Preventive Nutrition and Food Science
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• v.4 no.3
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• pp.171-174
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• 1999

For monitoring lipid oxidation development in cooked ground pork during refrigerationm, malonaldehydethiobarbituric acid(MA-TBA) contents were measured using high performance liquid chromatography(HPLC). As the oxidation proceeded during refergeration, TBA-reaction substances(TBARS) absorbances increased and the corresponding HPLC peak areas also increased proportationately. The correlation coefficient between the HPLC peak areas and MA-TBA absorbance were 0.9979. The treatemtn of cetrimide, an ion pairing agent, gave a complete resolution of the MA-TBA complex and the butanol extraction of the complex increased its recovery by 37.8%. Both cetrimide treatment and butanol extraction are essential steps for analyzing MA-TBA complex in ground pork wiht HPLC. A reliable and specific measurement of NA-TBA in ground pork was successfully performed using HPLC.

• Bulletin of the Korean Chemical Society
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• v.34 no.1
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• pp.139-142
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• 2013

A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

• Journal of Food Hygiene and Safety
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• v.16 no.1
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• pp.61-65
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• 2001

To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

• Analytical Science and Technology
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• v.37 no.2
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• pp.123-129
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• 2024

We present a rapid method for the determination of Cs, Sr, and Ba, heat generators found in highly active liquid wastes, by gas-pressurized extraction chromatography (GPEC) using a column containing a cation-exchange resin. GPEC is a microscale column chromatographic technique that uses a constant flow rate of solvent (0.07 mL/min) with pressurized nitrogen gas supplied through a valve. In particular, because this method uses a small sample volume (a few hundred microliters), it produces less chemical waste and allows for faster separation compared to traditional column chromatography. In this study, we evaluated the separation of Cs, Sr, and Ba using GPEC. The eluate from the column (GPEC or conventional column chromatography) was quantitatively analyzed using inductively coupled plasma-mass spectrometry to measure the column recovery and precision. The column reproducibility of the proposed GPEC system (RSDs of recoveries) ranged from 2.7 to 4.1 %, and the column recoveries for the three elements ranged from 72 to 98% when aqueous HCl was used as the eluent. The GPEC results are slightly different in efficiency and separation resolution compared to those of conventional column chromatography because of the differences in the eluent flow rate as well as the internal diameter and length of the column. However, the two methods had similar recoveries for Cs and Sr, and the precision of GPEC was improved by two-fold. Remarkably, the solvent volume required for GPEC analysis was five times lower than that of the conventional method, and the total analysis time was 11 times shorter.

• Bulletin of the Korean Chemical Society
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• v.25 no.10
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• pp.1489-1494
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• 2004

A gas chromatography/mass spectrometric assay method was developed for the determination of persistent organochlorine pollutants (POPs) in hair. For the exact extraction study was used hair of rat exposed with POPs. Sonication of the hair matrix with 3 M HCl solution in methylene chloride of the extraction methods studied was the most efficient and rapid sample preparation method. After sonication of rat hair was achieved clean up with a solid phase extraction procedure using silica gel-florisil. Elution was performed with 8 mL of methylene chloride. The eluate was concentrated to approximately 100 ${\mu}L$ and analyzed by gas chromatography-mass spectrometry (GC-MS). Detection limits of POPs were in the concentration range of 0.6-1.2 ng/g in rat hair. Aldrin, dieldrin, p,p-DDT and mirex were dosed rat for 4 weeks at concentration of 0.01 mg/L in drinking water and detected in rat hair at concentration of 2.8, 11.3, 7.9 and 15.6 ng/g, respectively. Aldrin and p,p-DDT were metabolized to dieldrin and p,p-DDE, which were detected in concentration of 9.7 and 2.9 ng/g in rat hair, respectively. The developed method may be valuable to be used to analyze POPs in human hair.