• Journal of Korean Society of Environmental Engineers
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• v.37 no.5
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• pp.262-268
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• 2015

This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.

• Korean Journal of Food Science and Technology
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• v.46 no.4
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• pp.425-431
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• 2014

In this study, the volatile compounds in 24 commercial Korean black raspberry wines were isolated by headspace solid-phase microextraction and analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 43 volatile components, including 15 esters, 12 terpenes, 7 alcohols, 4 acids, 3 ketones, and 2 aldehydes, were identified. Ethyl esters and alcohols such as ethyl acetate, ethyl octanoate, isoamyl alcohol, and phenethyl alcohol were the most represented groups among the quantified volatiles. In particular, various terpenes such as DL-limonene, linalool, alpha-terpineol, and myrtenol were identified. The differences in volatile components among the 24 black raspberry wines and possible sample grouping were examined by applying principal component analyses to the GC-MS data sets. The first and second principal components explained 43.9% of the total variation across the samples. No apparent sample groupings were observed according to manufacturing locations. The samples KU, BH, SR, and MO showed higher overall levels in the concentrations of terpenes originating from black raspberry, while other samples such as BB and HB, showed higher in ethyl ester and alcohol contents produced by yeast fermentation, respectively.

• Korean Journal of Environmental Agriculture
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• v.30 no.4
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• pp.419-423
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• 2011

BACKGROUND: Inorganic component is made up largely of salt, because the criteria are difficult to split into domestic and imported ingredients, organic examined the fatty acid composition is to see a possible use as a marker using gas chromatography-mass spectrometry (GC-MS). The 14 domestic samples and 8 imported samples were collected from China, India and other countries were investigated on item of 37 fatty acids. METHODS AND RESULTS: The major components were six species, myristic acid ($C_{14:0}$), palmitic acid ($C_{16:0}$), palmitoleic acid ($C_{16:1}$), stearic acid ($C_{18:0}$), oleic acid ($C_{18:2,n9}$), linoleic acid ($C_{18:2,n6}$) among detected twenty fatty acids including 9 unknowns. The content of palmitic acid were highest as 25.2 to 50.8% of total fatty acids contents. Domestic has seen the most amount of salt in the Taepyeong salts $250.8{\mu}g$/100g, imports $135.2{\mu}g$/100g salt in Chinese Weifang salts showed the lowest content. CONCLUSION(s): The total fatty acid content has seen the most amount of salt in 352.3 ug/100g Christmas island salts showed the lowest content of $164.0{\mu}g$/100g, as a result it is difficult to distinguish the domestic salts and imported by the composition of fatty acid.

• Analytical Science and Technology
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• v.23 no.2
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• pp.179-186
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• 2010

The oxidative metabolism of ibuprofen in healthy male urine collected at 3, 6, 9, 12 and 15 h after oral administration of ibuprofen was studied by GC/MS assay. To detect conjugated metabolites of ibuprofen, urine sample was acid-hydrolyzed with 6 M HCl at $100^{\circ}C$ for 30 min. To effectively extract ibuprofen and its metabolites, liquid-liquid extraction (LLE) was conducted at pH 3, 5, and 7, respectively. As a result, LLE at pH 3 was shown to be the best extraction condition. For the determination of trace amounts of ibuprofen and its metabolites in extract, trimethylsilylation (TMS) with BSTFA was applied and followed by GC/MS analysis. In this study, main 5 metabolites including parent drug were detected and these metabolites were assigned as three hydroxylated forms and one carboxylated form. Each metabolite was tentatively identified by both interpretation of mass spectrum and comparison with previously reported results. In addition, time profile of urinary excretion rate for parent drugs and metabolites was studied. Finally, the metabolic pathways of ibuprofen were suggested on the basis of the structural elucidation of its metabolites and excretion profiles.

• Journal of Food Hygiene and Safety
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• v.27 no.4
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• pp.332-338
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• 2012

A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.

• 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 Conservation Science
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• v.32 no.1
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• pp.21-32
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• 2016

Animal glue is a traditional material used extensively as adhesive and binder in mother-of-pearl, wooden structure, traditional painting, etc. Analysis of animal glue is usually performed with IR(infrared spectroscopy) based on the IR absorption of functional group. But, it has a limitation in confirming animal glue when a sample consists of several materials because of overlapping of the absorption band. Py/GC/MS(pyrolysis/gas chromatography/mass spectrometry) is a useful tool in analyzing the constituent of polymeric materials like animal glue by identifying their pyrolysate with very small amount of sample. In this study, confirmation of animal glue in a Dancheong sample was tried with this method. Characteristic pyrolytic compounds of animal glue and tung oil used in Dancheong were identified. Dancheong sample painted with Noerok as a coloring material, animal glue and tung oil was prepared and it was possible to find characteristic peaks of animal glue after thermal degradation and artificial weathering experiment. From this, we found that animal glue can be detected using py/GC/MS in cultural heritage samples consisting of several materials and in different condition. IR was also tried to analyze Dancheong sample and the results were compared with those of py/GC/MS for the detection of animal glue.

• Bulletin of the Korean Chemical Society
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• v.28 no.12
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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).

• Journal of Environmental Science International
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• v.15 no.5
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• pp.397-403
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• 2006

Compositional characteristics and origin of polycyclic aromatic hydrocarbons(PAHs), which should be strongly regulated for environmental protection in the crude oils and petroleum products, have been investigated by gas chromatography-mass spectrometry(GC/MS). In the crude oils analyzed, two-rings compound(naphthalene) of PAHs was detected around $72.3\sim93.5%$, but five- or six-rings compound of PAHs was not detected. In the crude oils analyzed, the molecular ratio indices of Phe/Ant(phenanthrene/anthracene)>15, Fla/Pyr(fluoranthene/pyrene)<1, BaA/Chr(benzo (a)anthracene/chrysene)$\leq0.4$ could be effectively applied, and we found that the origin of PAHs was petrogenic sources. Total PAHs concentrations in the crude oils were increased with increasing API gravity and with decreasing sulfur contents of the analyzed crude oils. Five- or six-rings compound of PAHs were not included in ail petroleum products except bunker-C. Furthermore, the molecular ratio indices of Phe/Ant(phenanthrene/anthracene) vs. Fla/Pyr(fluoranthene/pyrene) could be effectively applied as the standard for the PAHs contamination criterion at the other Korean areas.

• Analytical Science and Technology
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• v.16 no.6
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• pp.458-465
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• 2003

The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.