• Analytical Science and Technology
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• v.28 no.6
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• pp.436-445
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• 2015

Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.5
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• pp.783-789
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• 2000

This study was focused on the optimal extracting conditions of dimethyl-$\beta$-propiothetin as bioactive substance from green seaweed. Identification and quantification of dimethyl-$\beta$-propiothetin were measured by headspace gas chromatography after conversion to dimethyl sulfide by treatment with saturated NaOH solution. Dimethyl-$\beta$-propiothetin was extracted through various processes (solvent extraction, ultrasonication, boiling and autoclaving) from Ulva pertusa. The content of dimethyl-$\beta$-propiothetin extracted by autoclaving treatment showed higher than that of various extraction methods. Dimethyl-$\beta$-propiothetin content in extract of Ulva pertusa was 325,800 ng/g after autoclaving 121$^{\circ}C$ for 45 min. Dimethyl-$\beta$-propiothetin in exract of Ulva pertusa was comparative stable under low temperature. The retentions of dimethyl-$\beta$-propiothetin content in extract of Ulva pertusa were 76.6~99.8% by incubation at 10~6$0^{\circ}C$ for 2 hours. Chemical decomposition of dimethyl-$\beta$-propiothetin was observed under laboratory conditions at pH values higher than 9.5.

• Applied Biological Chemistry
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• v.34 no.2
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• pp.110-116
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• 1991

As the model compounds, citral and n-octanol which possess similar characteristics and structures of low molecular weight insect pheromones and $({\pm})-5-hydroxy-4-methyl-heptan-3-one$ which shows the aggregation pheromones activity of the rice weevil and the maize weevil were microencapsulated with low molecular weight polyethylene(LMPE) and urea-formaldehyde resin as wall materials. The core materials were microencapsulated as small particles in LMPE and urea-formaldehyde resin polymers and the microencapsulated polymers were white powders. And the polymer made from urea-formaldehyde resin was better than that from LMPE as wall material. The slow releasing effect and the releasing patten of the microencapsulated core materials were examined by solvent extraction method and headspace sampling method. Citral and n-octanol and $({\pm})-5-hydroxy-4-methyl-heptan-3-one$ were release more than 40 days and 15 days, respectively. The releasing pattern of urea-formaldehyde resin microcapsules showed rather smooth decrease than that of LMPE and was maintained at steady level longer.

• Journal of the Korean Society for Marine Environment & Energy
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• v.17 no.1
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• pp.27-35
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• 2014

The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

• Journal of Food Hygiene and Safety
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• v.28 no.3
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• pp.222-226
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• 2013

A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range $0.005{\sim}0.5{\mu}g/mL$, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice.

• The Korean Journal of Food And Nutrition
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• v.13 no.4
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• pp.334-341
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• 2000

The DMPT produced by marine algae is the main biogenic precursor of oceanic DMS. Also, DMPT is an efficient stimulant for growth, feeding, and body movement of fish and striped prawn, and appears to play a physiologic role as an osmoprotectant in algae. This study was focused on the extraction of dimethyl-$\beta$-propiothetin as bioactive substance from green seaweed. Identification and quantification of dimethyl-$\beta$-propiothetin were measured by headspace gas chromatography after conversion to dimethyl sulfide by treatment with saturated NaOH solution. Dimethyl-$\beta$-propiothetin was extracted through various processes(solvent extraction, ultrasonication, boiling and autoclaving) from Enteromorpha intesinalis. The content of dimethyl-$\beta$-propiothetin extracted by autoclaving treatment showed higher than those of various extraction methods. Dimethyl-$\beta$-propiothetin content in extract of Enteromorpha Enteromorpha was 311,200ng/g after autoclaving at 121$^{\circ}C$ for 60min. Dimethyl-$\beta$-propiothetin in extract of Enteromorpha intestinalis was comparatively stable under low temperature. The retentions of dimethyl-$\beta$-propiothetin content in extract of Enteromorpha intestinalis were 75.8 ~99.8% by incubation at 10~6$0^{\circ}C$ for 2 hours. Chemical decomposition of dimethyl-$\beta$-propiothetin was observed under laboratory conditions at pH values higher than 9.5.

• Applied Biological Chemistry
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• v.51 no.3
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• pp.238-244
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• 2008

The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.

• Analytical Science and Technology
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• v.25 no.6
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• pp.395-401
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• 2012

This study presents a method for the quantitative analysis of residual vinyl chloride monomer (VCM) in PVC products. In elution solvent, the extraction efficiency was similar by ethanol, THF, and acetone, but using n-hexane, it indicated relatively low extraction efficiency. Measuring VCM in the pulverized PVC samples, it showed reasonable results in both the direct injection method and headspace method with GC/MS. Regarding analysis of VCM in the intermediate sponge samples, five laboratories showed good results, and from the results, it was considered that VCM quantitative method in this study was reliable.

• Analytical Science and Technology
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• v.26 no.5
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• pp.299-306
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• 2013

Pyroligneous liquor as a byproduct from charcoal production of bamboo sprout produced damyang-gun has the broad benefits such as improvement of soil quality, plant growth control and is mainly used for the treatment of atopic dermatitis, fungi and many other skin diseases. In this study, flavor compounds of pyroligneous liquor from bamboo sprout produced in Damyang-gun were analyzed and compared using three different methods including direct analysis (DA), headspace solid phase microextraction (HS-SPME) and stir bar sorptive extraction (SBSE). Simultaneously, the analytical conditions of GC-MS for the determination of volatile compounds were optimized. Based on volatile organic compounds detected by GC-MS, SBSE and SPME methods showed higher sensitivity than direct analysis. Major compounds of pyroligneous liquor were cresol, guaiacol, p-ethyl guaiacol and syringol. These phenolic compounds are reported as the useful chemicals with medicinal activity.

• Korean journal of food and cookery science
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• v.14 no.5
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• pp.541-546
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• 1998

Volatile flavor components in leaf and petiole of fresh Pleurospermum kamtschaticum H$\_$OFFM/ were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the Rl of GC and mass spectrum of GC-MS. A total of 31 components, including 15 hydrocarbons, 4 aldehydes, 1 ketone, 5 alcohols, 2 esters, 3 acids and 1 oxide were identified in the essential oils. (Z)-${\beta}$-Farnesene, (Z, E)-${\alpha}$-farnesene and farnesene were the major volatile flavor components in fresh Pleurospermum kamtschaticum. Volatile flavor patterns of Pleurospermum kamtschaticum were analyzed using electronic nose. Sensor T30/1 and PA2 that were sensitive to alcohols had the highest resistance for fresh Pleurospermum kamtschaticum. Resistance of six metal oxide sensors was decreased in dried sample compared with fresh one.