• Journal of Environmental Health Sciences
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• v.28 no.4
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• pp.6-11
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• 2002

3.3'-Dichlorobenzidine(DCB) has be shown carcinogenic in several animals, and the development of non-invasive biomonitoring method in workers exposed with it is a very important subject. DNA adduct is a good biomarker for biomonitoring about carcinogens exposure, and lymphocytes is a good non-invasive samples. So we studied to analyze metabolites in blood lymphocytes of female Sprague-Dawley rats exposed orally with DCB(20, 30, and 40 mg/kg wt.) for 3 weeks. For analysis of them, we isolated DNA adducts from blood lymphocytes by using the enzymes method in /sup 32/P-postlabeling, and measured them by using gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM). 4-aminobiphenyl and phenanthrene-d/sub 10/ were added as internal standard for blank sample. Standard metabolites of DCB were synthesized with using pyridine and acetic acid which were promoter and controller in acetylation of DCB. And they were used for calibration curve. Our results showed two kinds of metabolites in DNA adducts of blood lymphocytes. They were N-acetyl 3,3'-dichlorobenzidine(acDCB) and N,N'-diacetyl 3,3'-dichiorobenzidine(di-acDCB ). They were combined with DNA at the same time as an acetyl of it was removed. So we measured DCB and acDCB for two kinds of metabolites in DNA adducts of blood lymphocytes. Our results showed the levels of DCB were 1.46∼2.26 times more than that of acDCB. And also the levels of metabolites in 20, 30 and 40 mg/kg wt. were gradually increased with going days from 1st to 3rd week. They are 1.66, 1.38 and 0.90 times in total metabolites, 1.76, 1.49 and 1.02 times in DCB, and 1.51, 1.22 and 1.28 times in acDCB. In conclusion, the results of this study showed DCB exposed to rats formed DNA adduct in blood lymphocytes after acetylated to N-acetyl 3.3'-dichloro benzidine(acDCB) and N,N'-diacetyl 3,3'-dichlorobenzidine(di-acDCB), and they could be analyzed by us ing gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM).

• Bulletin of the Korean Chemical Society
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• v.22 no.7
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• pp.685-688
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• 2001

A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of benzidine (BZ), N-acetyl benzidine (ABZ) and N,N-diacetyl benzidine (DABZ) in rat urine. BZ, ABZ and DABZ were extracted from urine at pH 8 with ethyl ether. Conjugated urinary metabolites were extracted at pH 8 after hydrolysis with 1 M HCl for 30 min at 100 $^{\circ}C.$ The dried extract was dissolved in 100 ${\mu}{\ell}$ of ethylacetate and then injected in gas chromatography-mass spectrometric (GC-MS) system without further purification or modification. BZ, ABZ and DABZ have good chromatographic properties and offer very sensitive response for the EI-MS (SIM) without any derivatization. The recoveries for BZ, ABZ and DABZ were about 98.0, 81.8 and 71.4%, respectively, at pH 8.0 and the concentration of 5.0 ng/mL. The coefficients of variation of BZ and ABZ were less than 9.5% from 0.1 to 100 ng/mL and that of DABZ was less than 13% in the same concentration range. The detection limits of the assay were 0.01 ng/mL for both BZ and ABZ, and 0.05 ng/mL for DABZ in urine or plasma 1.0 mL.

• Analytical Science and Technology
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• v.17 no.2
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• pp.130-144
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• 2004

Recently, the air pollution in A and B industrial area has become one of the most important issues, then 60 VOCs in the area were measured using a highly sensitive method. The VOCs were adsorbed onto Carbotrap using air sampler and subsequently desorbed by a thermal desorber system into gas chromatograph-mass spectrometry (TDS-GC-MS). The peaks of all compounds had good chromatographic properties and offered very sensitive response for the EI-MS (SIM). Method detection limits (MDL) ranged from 0.01 to 0.1 ppt(v/v), and linearities of calibration curves were over 0.995. We analyzed total 90 atmosphere air samples of A and B industrial complex using the method. Benzene, toluene, ethylbenzene, xylene, n-hexane, fluorotrichloromethane, carbon tetrachloride, 1,2-dichloroethane, 1,1,1-trichloroethane, trichloroethylene, tetrachloroethylene, styrene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene, sec-butylbenzene and naphthalen were identified as the major compounds in the air, and their average concentrations were 0.81, 5.02 1.30, 3.0, 0.81, 37.9, 0.07, 0.15, 0.15, 0.79, 0.06, 0.33, 0.03, 0.12, 0.23, and 0.35 ppb(v/v), respectively. The concentrations of VOCs were low in summer and high in fall or winter. When the concentrations detected in air compare with WHO's norm, no case exceed it.

• Korean Journal of Food Science and Technology
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• v.30 no.4
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• pp.721-727
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• 1998

An analytical method for simultaneous and rapid determination of organophosphorus, organochlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The analysis is performed by gas chromatograph with mass selective detector (GC/MSD) in selected ion monitoring (SIM) mode. Pesticides were extracted from samples with acetone by automated Soxhlet apparatus and this extract was evaporated to dryness for the analysis. The residue was dissolved in hexane, followed by a treatment with a Sep-Pak florisil catridge. Pesticides were positively confirmed by GC/MS, retention times, and ion ratios. This analytical method allows a rapid, reliable, and a good recovery of hydrophilic pesticides. Except far captafol, captan, dichlofluanid and dichlorvos, recoveries of 42 pesticides were over 70%.

• Korean Journal of Food Science and Technology
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• v.27 no.6
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• pp.921-927
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• 1995

Peach pulp was separated into serum and insoluble pulp by centrifugation at 11,000 rpm for 10 min. The serum portion was concentrated at $50{\sim}55^{\circ}C$ and $30{\sim}50\;mmHg$ with aroma recovery. Vapor generated at the early stage of vacuum evaporation was condensed and taken as aroma fractions: AR-1($0{\sim}5%$), AR-2($5{\sim}10$), AR-3($10{\sim}15%$), AR-4($15{\sim}20%$). Dynamic headspace concentration method was used to trap volatile compounds in aroma fractions and identification of aroma compounds was made by GC/MS. The yield of serum separated from peach pulp was 70.5% and the serum fraction contained the most of aroma compounds. Thirty-one aroma compounds, including ethylene, benzaldehyde, l-limonene and ${\gamma}-dodecalactone$ were identified. The efficiency of aroma recovery was reduced, as the recovery time was extended, as indicated by less peak numbers and peach areas of aroma fractions.

• Analytical Science and Technology
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• v.11 no.5
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• pp.321-331
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• 1998

The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAHs) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some extraction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAHs was possible by partial variation of oven temperature of GC/MS in temperature range $80{\sim}310^{\circ}C$. Extraction procedures of PAHs in water samples were somewhat modified and compared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAHs were 71.3~109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7~94.9%) were obtained in case of $C_{18}$ disk extraction method by filtration. And extraction recoveries of PAHs by $C_{18}$ solid-phase were in the range of 51.8~77.9%. Method detection limits (S/N=5) of 19 PAHs were in the range of 0.25~6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05~1.25 ppb by disk extraction methods.

• Journal of Ecology and Environment
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• v.29 no.4
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• pp.381-387
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• 2006

We analyzed the total yields and composition of essential oils in leaf extracts of Nepeta cataria by Gas Chromatography Mass Spectrometry (GC-MS). Thirty-six compounds representing 97.0% of total oil were detected. The major constituents of essential oils in Nepeta cataria were nepetalactone (90.9%), unidentified compound (Retention time 17.35; 1.82%), 1,8-cineol (1.49%), ${\beta}-caryophyllene$ (1.12%), and ${\beta}-pinene$ (1.078%). The volatile compounds in leaf extracts of N. cataria concentrated to nepetalactone ($88.83{\sim}93.33%$) remarkably. In the essential oil of N. cataria cis,trans-nepetalactone ($30.2{\sim}37.8%$) and cis,cis-nepetalactone ($31.5{\sim}37.0%$) were found as the main constituents. The effects of essential oil of N. cataria on the growth of six microorganisms (Bacillus cereus, B. subtilis, B. amyloliquefaciens, Escherichia coli, Staphylococcus aureus subsp. aureus, and Pseudomonas aeruginosa) were investigated. The essential oil of N. cataria had strong inhibitory effect on the growth of three fungal species (Bacillus cereus, B. subtilis, and B. amyloliquefaciens). The essential oil from N. cataria was found to have a low antimicrobial activity against Staphylococcus aureus subsp. aureus, while no activity were found against Escherichia coli and Pseudomonas aeruginosa. Results indicate the significant antimicrobial effect, which may be depended on the yield of nepetalactone.

• Journal of the Korean Society of Tobacco Science
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• v.29 no.2
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• pp.118-124
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• 2007

GRLs(Guidance Residue Levels) of agricultural chemicals for tobacco are recommended by the CORESTA Agro-Chemical Advisory Committee guide. In the GRLs list, organochlorine group is one of pesticides commonly used on tobacco cultivation. In this model study, the quantitative correlation in the transfer rate of pesticide residue into tobacco smoke by spiking of organochlorine pesticides to cigarette and pyrolysates were investigated. The spiking concentration referred to the range of GRLs list and the organochlorine pesticides in mainstream smoke were analyzed by GC-MS. For the understanding of the composition variation versus temperature, the behavior of pesticides was investigated by pyrolysis-gas chromatography-mass spectrometry(Py-GC-MS). In this study, the transfer rate of pesticide residue into tobacco smoke at four different spiking concentration and the composition of pyrolysates were analyzed differently. At $10\;{\mu}g/cig$ spiking concentrations, the organochlorine pesticides were transferred into tobacco smoke in $0.02\;{\sim}\;10.19\;%$ each of component and the most of pesticides were pyrolyzed during smoking. It was found that the decomposition compounds from organochlorine pesticides were mainly composed of oxygenated and nitrogenous compounds. This study could estimate that the transfer rate of pesticides into tobacco smoke is very small amount.

• Analytical Science and Technology
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• v.16 no.6
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• pp.483-487
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• 2003

Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.

• Analytical Science and Technology
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• v.13 no.3
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• pp.385-393
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• 2000

A gas chromatography-mass spectrometric (GC/MS) procedure for the determination of amineptine (dihydro-10, 11-dibenzo[a, d] cycloheptenyl-5-amino-7-heptanoic acid) and its main metabolites in human urine was described. Amineptine has been known to be extensively metabolized by the ${\beta}$-oxidation of the heptanoic side chain with formation of pentanoic side chain metabolite ($C_5$-metabolite), and lactamizarion by internal dehydration of (${\beta}$-oxidized metabolite (${\delta}$-lactam). The detection of these compounds was based on acid hydrolysis, liquid-liquid extraction and trimethylsilylated derivatization of the carboxylic acid group. For the determination of amineptine and its metabolites in biological fluids, selected ions at the m/ 192, molecular ion and one of the characteristic ions were monitored by GC/MS. On the excretion study of amineptine in human urine, 70-90% of amineptine, ${\delta}$-lactam, and $C_5$-metabolite were found to be excreted within 4 hours and their excretion completed within 20 hours.