• Analytical Science and Technology
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• v.34 no.1
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• pp.23-35
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• 2021

In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

• 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 Korean Society of Environmental Engineers
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• v.32 no.2
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• pp.155-164
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• 2010

Emission from biomass combustion such as meat charbroiling is an important source of organic aerosol. Since source profiles are necessary input profiles for source apportionment of aerosol by a chemical mass balance model, meat cooking organic source profiles are developed by measuring organic marker compounds, including palmitic acid, stearic acid, oleic acid and cholesterol as well as PAH compounds. Emissions from meat and pork charbroiling are collected on quartz filters with a PM10-high volume sampler, extracted with organic solvents, derivatized with diazomethane/TMS and analyzed by GC/MS isotope dilution method. Organic and elemental carbon are also analyzed by an OCEC analyzer. Wt.% of cholesterol to the organic carbon(OC) content from beef and pork charbroiling is only 0.056 and 0.062, but wt. % of all saturated fatty acids to the OC content from beef and pork charbroiling is 2.727 and 2.022, and the wt% of all unsaturated fatty acids to the OC content is 0.278 and 0.438, respectively. Content of total PAH compounds to the OC content from beef charbroiling is higher than that from pork charbroiling, and those are 0.116 wt% and 0.044 wt%. Among PAH compounds benzo(a)pyrene as a single compound is account for 0.0071 wt% and 0.0023 wt% of OC content from beef and pork charbroiling. Ratios of marker compound to cholesterol are calculated, and those values are in good agreement with the values already reported at the food cooking emission, indicating that they can be used as organic source profiles for the apportionment of organic aerosol.

• Analytical Science and Technology
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• v.19 no.1
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• pp.73-85
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• 2006

Blood serum concentrations of polychlorinated biphenyls (PCBs) were measured in employees who worked at a municipal solid waste incinerator (MSWI), members of residential community who lived near the MSWI (<0.3km) and members of residential community lived far from the MSWI (>10 km). Human blood serum samples were analyzed for all PCB congeners using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS). The mean levels of total PCBs and dioxin-like PCBs in 87 serum samples were 242.77 ng/g lipid and 8.83 TEQ pg/g lipid, respectively. The PCB homologue profiles showed that penta-, hexa-, hepta-chlorinated biphenyls contributed more than 80% of the total PCBs concentration. The most abundant congeners were PCB153, PCB138, PCB180, PCB187, PCB118. A statistical analysis was performed to determine whether there were significant correlations between PCB concentrations and specific variables such as age, gender, smoking habits, occupation, BMI (Body Mass Index) and time of residence. As a result, the age was found to be strongly correlated with serum PCB concentrations. In addition, there were strong correlations between total PCBs and PCB153 (r=0.93, p<.0001), dioxin-like PCBs and PCB118 (r=0.98, p<.0001). So these two congeners are satisfactory indicators for total PCB concentrations and dioxin-like PCBs in human blood respectively.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.157-163
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• 2012

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

• Korean Journal of Food Science and Technology
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• v.52 no.5
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• pp.524-528
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• 2020

The aim of this study was to enhance the use of wheat bran in lactic acid bacteria (LAB) fermentation. LAB fermentation of wheat bran and the flavor components and amino acids of fermentation products were analyzed using gas chromatography-mass spectrometry (GC/MS) and high-performance liquid chromatography (HPLC). The results showed that total flavor components increased by 93% and 73% in the animal-based LAB mixture (T2) and plant-based LAB mixture (T3), respectively, after fermentation. Among these components, 2,3-butanedione (diacetyl), known for its buttery flavor, was detected at concentrations of 18.44 ng/g (T2) and 16.95 ng/g (T3). Levels of hexanal and nonanal, which causes off-flavor components in wheat bran, dramatically decreased after T2 fermentation; similarly, levels of total free amino acids decreased by 37.6% (T2) and 36.7% (T3) after fermentation. This may explain why some components were bound to volatile compounds during LAB fermentation. These results suggest that LAB-fermented wheat bran is a potential value-added food material.

• The Plant Pathology Journal
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• v.33 no.5
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• pp.499-507
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• 2017

In an attempt to develop a biological control agent against mycotoxigenic Fusarium species, we isolated Bacillus amyloliquefaciens strain DA12 from soil and explored its antimicrobial activities. DA12 was active against the growth of mycotoxigenic F. asiaticum, F. graminearum, F. proliferatum, and F. verticillioides both in vitro and in planta (maize). Further screening using dual culture extended the activity range of strain DA12 against other fungal pathogens including Botrytis cinerea, Colletotrichum coccodes, Endothia parasitica, Fusarium oxysporum, Raffaelea quercus-mongolicae, and Rhizoctonia solani. The butanol extract of the culture filtrate of B. amyloliquefaciens DA12 highly inhibited the germination of F. graminearum macroconidia with inhibition rate 83% at a concentration of $31.3{\mu}g/ml$ and 100% at a concentration of $250{\mu}g/ml$. The antifungal metabolite from the butanol extract was identified as iturin A by thin layer chromatography-bioautography. In addition, volatile organic compounds produced by DA12 were able to inhibit mycelial growth of various phytopathogenic fungi. The volatile compounds were identified as 2-heptanone, 5-methyl heptanone and 6-methyl heptanone by gas chromatography-mass spectrometry (GC-MS) analysis. These results indicate that the antagonistic activity of Bacillus amyloliquefaciens DA12 was attributable to iturin A and volatile heptanones, and the strain could be used as a biocontrol agent to reduce the development of Fusarium diseases and mycotoxin contamination of crops.

• Korean Journal of Soil Science and Fertilizer
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• v.38 no.1
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• pp.25-31
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• 2005

A soil bacterium, Bacillus subtilis HJ927, exhibiting strong antagonistic property against pathogenic fungi was isolated from pepper fields infested with Phytophthora capsici. Pepper plants inoculated with P. capsici revealed severe root mortality while plants co-inoculated with B. subtilis HJ927 and P. capsici showed drastically reduced root mortality. Low molecular weight substances released by B. subtilis HJ927 mediated the plant protective effect. The anti-fungal compounds released by B. subtilis HJ927 were identified as 3-methylbutyric acid, 2-methylbutyric acid, and methyl 2-hydroxy, 3-phenylpropanoate by high-performance liquid chromatography and gas chromatography-mass spectrometry. In addition to these compounds, B. subtilis HJ927 also produced ${\beta}$-1,3-glucanase, a hydrolytic enzyme implicated in antifungal activity.

• Food Science and Preservation
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• v.13 no.3
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• pp.351-356
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• 2006

This study was carried out to investigate the change of functional component and volatile flavor components from garlic for which both were treated with protopectinase (PPase) and mechanical maceration during storage period. Alliin content of gallic suspensions macerated mechanically were 11.0 mg/g at 0 day and 6.6 mg/g at 24 day. Whereas alliin content of garlic treated with PPase were 8.5 m/g at 0 day and 7.0 mg/g at 24 day. Importantly, over 40% of alliin which is the most unstable component during the mechanical maceration remained with an intact form for 24 day after the enzymatic treatment. The flavor component from gallic suspensions were extracted by solid-phase microextraction (SPME) and were analyzed and identified by gas chromatography (GC) and chromatography/mass spectrometry (GC/MS). The number and concentrations of flavor components of gallic macerated mechanically were increased during storage period, and total 18 kinds of flavor compounds were identified. Thus, the PPase treatment of garlic could be a better choice for preparation of the highly valuable and functional processed food as well as for prolonging the preservation period.

• Korean Journal of Food Science and Technology
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• v.28 no.5
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• pp.827-833
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• 1996

Along with the increased necessity for an efficient utilization of Korean wild edible plants growing in fields and mountains, attempts were made to investigate the patterns of flavor changes accompanied hy various conditions of dispersion medium. The effect of various pH values and concentration of sucrose or NaCl of dispersion medium on volatile flavor patterns was investigated to evaluate the applicability of flavor components extracted from Capsella bursa-pastoris for food industry. Essential oils from this wild plant were isolated by simultaneous steam distillation-extraction (SDE) method using diethyl ether as solvent. Concentrated samples were analyzed s chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Most volatile flavor components of Capsella bursa-pastoris showed good recovery when steam distilled at pH 7 by SDE method. Increasing concentration of sucrose and 15% by NaCl, resulted in greater numbers of identified flavor components from Capsella bursa-pastoris.