• Analytical Science and Technology
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• v.13 no.5
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• pp.666-674
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• 2000

The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

• Analytical Science and Technology
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• v.23 no.4
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• pp.395-404
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• 2010

A multi-residual method using gas chromatography coupled with mass spectrometry (GC/MS/ MS) was developed for the analysis of 105 pesticides. This method was tested on lemons, beans and other vegetables. The pretreatment of these pesticides was performed by liquid-liquid partition followed by cleanup with solid phase extraction cartridge (SPE Florisil), after acetonitrile extraction from matrices and sodium chloride (15 g) addition. The recovery ranged from 71.1% to 126.0% except for azinphosmethyl, famoxadone, fenamidone, flufenoxuron and triadimefon in lemons and from 72.5% to 124.5% in bean. In lemon, the limit of detection (LOD) and limit of quantification (LOQ) were 0.001~150 ng/ mL and 0.004~500 ng/mL, respectively.

• Korean Journal of Food Science and Technology
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• v.28 no.3
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• pp.421-427
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• 1996

Ethyl carbamate is an animal carcinogen and a suspected human carcinogen found in fermented foods and beverages. For the determination of ethyl carbamate in typical Korean diet, an analytical method was established for the food as complex as Kimchi. Kimchi samples collected from various locations in the country were homogenized and extracted four times with ethyl acelate. Following concentration and reconstitution with water, the extract was loaded onto $C_{18}$ column. Fraction containing ethyl carbamate was eluted with methanol, while most of the red pigment of the sample was retained on the column. The eluent was further purified with alumina, followed by Florisil column. The final eluent was analyzed by gas chromatography mass spectrometry in the selected ion monitoring mode. None of the twenty Kimchi samples showed ethyl carbamate level higher than 4.6 ppb without correction for the recovery. The concentration of ethyl carbamate in Kimchi increased as pH decreased, suggesting fermentation dependent formation of ethyl carbamate.

• Korean Journal of Food Science and Technology
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• v.29 no.3
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• pp.427-431
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• 1997

A simultaneous and rapid gas chromatographic determination of organophosphorus, organo-chlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The pesticides were extracted from samples with acetone by automated soxhlet apparatus and this extract was evaporated to dryness. The residue was dissolved in hexane, the solvent was applied to a Sep-Pak florisil catridge, was eluted with 50% ethyl acetate in n-hexane, and was injected to dual GC-ECD/NPD system. This simple method affords a high recovery of hydrophilic pesticides, allows rapid analysis, and is cheap to perform. Except for dichlorvos and captan, recoveries of 46 pesticides were over 60%.

• Korean Journal of Food Science and Technology
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• v.30 no.3
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• pp.517-522
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• 1998

Hydrocarbons in soybeans were analyzed to determine whether the hydrocarbons can be applied for detecting post-irradiation of soybeans. Yellow and green soybeans were irradiated at 0.5, 1, 3, and 6 kGy. Fats were extracted with hexane and then hydrocarbons were separated from the fat through Florisil column. The hydrocarbons were analyzed with GC. Hydrocarbons 17:2, 16:3, 17:1, and 16:2 were detected in the samples irradiated at 0.5 kGy or higher, but not in the unirradiated ones. The detection levels of hydrocarbons increased with the dose of the irradiation. When unirradiated or irradiated soybeans were roasted or boiled, these hydrocarbons were detected in the samples irradiated at 1 kGy or higher, but not in the unirradiated ones. A blind test confirmed that the hydrocarbon determining method could detect the soybeans irradiated at 1 kGy.

• Analytical Science and Technology
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• v.17 no.1
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• pp.29-36
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• 2004

An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

• 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%.

• Journal of the Korean Society of Food Science and Nutrition
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• v.30 no.5
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• pp.770-776
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• 2001

To compare chemical properties of irradiated legumes (soybean, peanut, red bean, mung bean) produced in Korea and China, radiation-induced hydrocarbons from the samples were investigated. The legumes were gamma-irradiated at 0.5, 1, 2 and 4 kGy, from which lipid was extracted with hexane. Hydrocarbons were separated by florisil column chromatography and then analyzed with GC-MS method. The chromatograms of irradiated samples showed several radiation-induced hydrocarbons, which were affected by the fatty acid compositions of legumes. Hydrocarbons, such as 1, 7, 10-hexadecatriene (16:3),6,9-heptadecadiene (17 : 2), 1, 7-hexadecadiene (16 : 2) and 8-heptadecene (17 : 1), were predominantly detected in soybean, peanut and red bean irradiated at 0.5 kGy or above, whereas 17 : 1 was not found in mung bean. The detected amount of hydrocarbons increased with irradiation doses. There is no apparent difference in qualitative and quantitative profiles of the corresponding hydrocarbons depending on the origin of legumes.

• Preventive Nutrition and Food Science
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• v.3 no.4
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• pp.339-343
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• 1998

Gamma-irradiated chicken at dose levels of 0.1 to 10 kGy was subjected to detection of radiation-induced hydrocarbons whether irradiated or not. The hydrocarbons extracted from chicken fat were separated by florishil column chromatography and identified with GC-FID and GC/MS methods. Eight kinds of hydrocarbons were identified from irradiated chicken, among which 1, 7-hexadecadiene and 8-heptadencene were detected as major compounds , Remarkably radiation-induced hydrocarbons in irradiated chiken were detected at 0.5kGy and over. The concentration of radiation-induced hydrocarbons was relatively constant during 16 weeks.

• Journal of Environmental Science International
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• v.15 no.3
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• pp.229-236
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• 2006

Organophosphorus pesticides (OPPs) contents in the sewage sludge derived from the residential and industrial areas were determined in order to characterize contemporary organic contamination levels as a part of the ongoing development of the environmentally sound sewage sludge management strategy in Korea. OPPs were extracted from freeze-dried sludges in a ultrasonic extractor. The extracts were cleaned-up by florisil column and subsequently fed into gas chromatograph/nitrogen phosphorus detector (GC/NPD) for determining OPP contents. Diazinon, dimethoate, disulfoton, EPN, malathion, methyl parathion, parathion, phorate and sulfotep were present in the appreciable amount in the domestic sewage sludges. The sum of the 9 OPPs in the sewage sludge varied from 534.8 to 15552.1 ${\mu}g/kg$, dry wt..