• Analytical Science and Technology
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• v.22 no.2
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• pp.119-127
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• 2009

This study was carried out to investigate the distribution characteristics of persistent organic pollutants in incineration residues at industrial waste incinerators and municipal solid waste incinerators, which were analyzed by the official analytical method for the endocrine disrupting chemicals and the waste. Seven of 12 persistent organic pollutants were quantitatively analyzed by GC-MSD (SIM-mode). Hexachlorobenzene was detected in 21 samples among 44 incineration residues. The level of hexachlorobenzene was 0.132-8.138 ng/g in incineration residues, 0.195-5.765 ng/g in fly ash at industrial waste incinerators, 0.270-1.828 ng/g in bottom ash and 0.154-50.643 ng/g in fly ash at municipal solid waste incinerators, respectively.

• Analytical Science and Technology
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• v.23 no.2
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• pp.187-195
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• 2010

To assess health risk for the intake among residents after the Hebei Spirit oil spill, 16 Polycyclic Aromatic Hydrocarbons (PAHs) in seafood samples from oil contaminated bay were determined by Gas Chromatography-Mass Spectrometry (GC-MSD) and samples were personally collected and purchased by residents. Samples were hydrolyzed with KOH and extracted with methylene chloride. The extracted solution were cleaned up using silica/florisil column and 16 PAHs were eluted by methylene chloride : n-hexane (1:9) mixture and determined by GC-MSD in Selected Ion Monitoring (SIM) mode. The mean recoveries for 16 PAHs ranged from 79% to 85%. The 16 PAHs levels in 126 samples ranged from 0.17 to $6.04\;{\mu}g$/kg and the TEQBaP (Toxic EQuivalents) levels in 126 samples were calculated using benzo(a)pyrene toxic equivalency factor for individual 16 PAHs and ranged from 0 to $0.91\;{\mu}gTEQ$/kg. The average Benzo(a)pyrene dietary exposure of residents was $5.5{\times}10^{-8}\;mg/kg$ bw/day and the average PAHs chronic dietary exposure was $1.3{\times}10^{-5}\;mg$ TEQ/kg bw/day. The margin of exposure (MOE) and the excess cancer risk and were $1.8{\times}10^6$ and $9.8{\times}10^{-8}$, respectively. Therefore, the assessment result was considered as low concern for health risk.

• Journal of Food Hygiene and Safety
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• v.5 no.3
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• pp.159-164
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• 1990

To detect and quantitation residual antibiotics and antibacterial agents in meats, we performed a biological assay employing the three microorganisms Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778 for the screening purpose and developed a Gas Chromatography-mass Spectrometry(GC/MS) analysis for the confirmation and quantiation. In the biological assay (paper disk method), three test solution are used depending on the character of the residual antibiotics and antibacterial agents, follow by a simple clean up procedure which includes homogenization with Mcilvaine buffer, defatting with includes homogenization with Mcilvaine buffer, defatting with hexane, extraction with chloroform, clean-up by Sep-Pak $C_{18}$ and Bakerbond SPE carboxylic acid column. The chloroform layer is used for the analysis of sulfa agents. macrolides antibiotics and antibacterial agents, Adsorbed materials in the Sep-Pak $C_{18}$ were also employed for th analysis of penicillins and tetracyclines. Effluents from the Sep-Pak $C_{18}$ were cleaned-up one more by Bakerbond 10 SPE COOH column and employed for the analysis of aminoglycosides. In the instrumental analysis by using the GC/MSD, residual antibiotics and antibacterial agent were quantitated by selected ion monitoring (SIM) mode after derivatization. A simultaneous analysis of six residual antibiotic and antibacterial agent such as oxytetracycline, penicillin, ampicillin, choliraphenicol and thiamphenicol was developed with simple cleanup procedures revealing good recovery and reproducibility. Also, simultaneous detection of macrolides antibiotics such as erythromycin, spiramycin, and oleandomycin was developed after acid hydrolysis due to their large molecular structures. Because of the high reproducibility and selectivity of these two methods, it is very desirable that the combination of the two methods be used in the bioassay for the screening of residual antibiotics and antibacterial agent and that GC/MSD analysis be used for the confirmation and quantitation.

• Korean Journal of Medicinal Crop Science
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• v.10 no.3
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• pp.206-211
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• 2002

For developing natural presevatives, essential oils of Mentha arvensis L. var. piperascens Malivaud and Agastache rugosa O. Kuntze were analyzed the composition of two oils and experimented on microorganism survival. Main components of Mentha arvensis oil were isomenthol (26.84%) and menthol (25.48%), and those of Agastache rugosa oil were estragole (79.83%) and limonene (4.13%) from GC-MSD analysis. Inhibition activities of Mentha arvensis oil against growth of Escherichia coli O157 : H7 ATCC 43895 and Salmonella typhimurium ATCC 7988 were observed from their clear zone $(9{\sim}14 mm\;&\;9{\sim}13\;mm)$, and that of Agastache rugosa oil were done from the clear zone $(13{\sim}20 mm\;&\;10{\sim}18\;mm)$ by concentration-dependent manner, respectively. In the inhibition test on CFU/ml of the microorganisms, both of the plant essential oils at concentration of 5 and 10 mg showed potent growth inhibition activities from 9 hour of incubation. Analysis using transmission electron microscope on E. coli also showed antimicrobial activities of the oils as deformation of the cell and loss of the intracellular materials.

• Journal of Environmental Science International
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• v.15 no.8
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• pp.811-817
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• 2006

We were carried out to monitor pesticide residues in herbal medicine. In Korea Pharmacy, these are no critics for pesticides except 5 kinds of organic chlorines (BHC, DDT, Aldrin, Endrin, Dieldrin) and heavy metals. We analysed 53 kinds of pesticides consisted of 14 kinds of organochlorines, 20 kinds of organophosphoruses, and 19 kinds of pesticides estimated endocrine disruptor on 373 samples consisted with 30kinds of herbal medicine. In this study, Domestic, Chinese and Japanese herbal medicines were tested with GC/ECD, GC/NPD and then confirmed with GC/MSD. Recoveries were 75$\sim$l10% in ECD detector and 76$\sim$97% in NPD detector. Detection limits were 0.004$\sim$0.064ppm in ECD detector and 0.006$\sim$0.094ppm in NPD detector. Organochlorines and others were not detected in samples.

• Proceedings of the Korean Society of Food Hygiene and Safety Conference
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• 2001.10a
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• pp.140-140
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• 2001

A sensitive analytical method based on gas chromatograpy-mass spectrometry with a selected ion monitoring (GC/MS-SIM) with the purge-and-trap concentration and with headspace method (in limited applications) was developed for determining of epichlorohydrin in canned beverages coated with epoxy resin. The calibration curve in the range of $0.5\sim50ng$ had correlation coefficient greater than 0.998 and a detection limit of $0.l\mug/L$ was obtained using a sample volume of 20ml. The predominant ions of epichlorohydrin produced in MSD using electron ionization(EI) were m/z 57 ([M-CI]+) and 62/64 $([M-CH_2O]+)$. In survey of epichlorohydrin in thirty commercial canned beverage samples, none of them was detected.

• Korean Journal of Food Science and Technology
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• v.34 no.3
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• pp.385-389
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• 2002

Analytical method for diethylstibestrol (DES) and zeranol, which are growth promoters, in muscle foods was studied. Through selected ion monitoring analysis by GC-MSD for hormones, $M^+$ 412, 420, 416, and 433 for DES, $D_8DES$, ${\beta}-estradiol$, and zeranol, respectively, were selected for quantitative analysis. Removal of interferences in meat was done by passing the meat through 1 cc of strong anion exchanges resin, Dowex $2{\times}8$, 400 mesh, whereby the recoveries of DES and zeranol were achieved. Recoveries of DES and zeranol were ranged from 85 to 110%, and 75 to 110%, respectively, in meat using $D_8DES$ as an internal standard, while were 82 to 105%, and 65 to 120%, respectively, using ${\beta}-estradiol$ as an internal standard. These results show that both $D_8DES$ and ${\beta}-estradiol$ can be adopted as the internal standard for the analysis of DES and zeranol in muscle foods. Limits of detection of DES and zeranol were 0.05 and 1.0 ng/g, and limits of quantitation were 0.5 and 1.0 ng/g, respectively. The results of this study revealed no DES and zeranol were present in 14 samples of beefs, porks, ducks, chickens, mutiplicated flat fish, and trout.

• Journal of Environmental Science International
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• v.15 no.7
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• pp.669-676
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• 2006

PAHs are major pollutants that are widely distributed in soil and groundwater environment, so that may be regarded as carcinogens. We investigated the degradation kinetics of PAH in aqueous solution when low pressure UV energy and ultrasonic irradiation were applied. Phenanthrene and pyrene were used as model compounds. The degrees of degradation of these compounds with time were analyzed with a GC/MSD (SIM-mode). UV photolysis experiments showed that phenanthrene was reduced by 90 -67% at initial concentrations of 1 ppm to 8ppm whilst it decreased to 50% at 10 ppm. Under the same conditions pyrene was degraded up to about 75% at lower initial concentrations but the reduction efficiency dropped to a level of 34 to 29% at the higher concentrations above 8 ppm. The reaction orders for phenanthrene and pyrene were found to be zero-th and ca. -0.4th order, respectively, thus implying that the reported assumption of pseudo 1st order reaction for some PAHs would be no longer valid. PAH degradation was roughly proportional to the intensity of UV (number of lamps), exhibiting maximum 92.5% of the degradation efficiency. The solution pH was lowered to 4.4 from 6.4 during the experiments partially because the carbons decomposed by the energy reacted with oxygen radicals to produce carbon dioxides. Ultrasonic irradiation on phenanthrene solutions gave relatively poor results which matched to 50 to 70% of degradation efficiency even at 2 ppm of initial concentration. Phenanthrene was found to be degraded more efficiently than pyrene for the two energy sources. Ultrasound also followed the same reaction kinetics as UV energy on PAH degradation.

• Analytical Science and Technology
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• v.27 no.6
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• pp.339-346
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• 2014

The author assessed the availability of urine reference material for proficiency test provided for laboratories in occupational health. N-methylacetamide is the biomarker of exposure to N,N-dimethyl acetamide, which was used as the substitute for hepatotoxic N,N-dimethylformamide (DMF). N-methylacetamide (NMAC) urine samples of 3 different levels covering the 0.2~2 times of the exposure limit were tested. Stability test up to 180 days (0, 7, 30, 60, 180 days) at 4 different temperatures (-60, -20, 5, $25^{\circ}C$) and homogeneity test were performed for these samples. New analytical condition by GC/MSD using SIM mode (m/z 58, 59) and DB-624 column was investigated for better selectivity, sensitivity and resolution. Urinary NMAC samples showed good homogeneity for 3 levels. These samples also showed good stability up to 180 days. The data of stability and homogeneity of urinary DMAC confirmed the basis of including this item into Korean proficiency test for occupational health laboratories since 2008.

• Korean Journal of Food Science and Technology
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• v.31 no.5
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• pp.1221-1226
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• 1999

Volatile flavor components of glutinous rice koji kochujang made by an improved method were analyzed by using a purge and trap method during fermentation and identified with GC-MSD. Twenty-one volatile flavor components detected immediately after making kochujang including 6 alcohols, 6 esters and 2 aldehydes. Forty-six volatile flavor components including 15 alcohols, 15 esters, 5 acids, 5 aldehydes, 1 alkane, 1 amine, 1 alkene and 3 others were found in an improved kochujang after 150 day of fermentation. Twenty kinds of flavor components, 5 alcohols such as ethanol, 3-methyl-1-butanol. 2-methyl-1-propanol, 6 ester such as ethyl acetate. 2-methylpropyl acetate, ethylbutanoate, phenylacetate, 2 aldehydes and 7 others were commonly found through the fermentation period. Peak area(%) of ethenone was the highest one among the volatile flavor components at immediately after mashing, and ethyl acetate showed the highest peak area after $30{\sim}60$ day of fermentation, and ethanol showed the highest peak area after $90{\sim}120$ day of fermentation, and 3-methyl-1-butanol showed the highest peak area after 150 day of fermentation(as major components). 2-Methyl-1-propanol, 1-butanol and methylbenzene were detected in glutinous rice koji kochujang during the fermentation.