• Korean Journal of Food Science and Technology
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• v.35 no.6
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• pp.1072-1078
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• 2003

Radiation-induced hydrocarbons and 2-alkylcycolbutanones are formed from the fatty acids of irradiated fat. These radiation-induced compunds were detected by fat extraction with a Soxtec apparatus from dried cuttle fish (Sepia officinalis), isolation of hydrocarbons and 2-alkylcyclobutanones with florisil column chromatography, and identification of GC/MS. Concentration of hydrocarbons produced by -λ-irradiation depended on the composition of fatty acid in dried cuttle fish. The major hydrocarbons in the irradiated dried cuttle fish samples were pentadecane and 1-tetradecene from palmitic acid, heptadecane and 1-hexadecene from stearic acid, and 8-heptadecen and 1,7-hexadecadiene from oleic acid. Of 2-alkylcyclobutanones, 2-dodecylcyclobutanone from palmitic acid was present at the highest level in irradiated dried cuttle fish. The radiation-induced hydrocarbons and 2-alkylcyclobutanones from the irradiated dried cuttle fish were detected at 0.5 kGy and over, but not detected in the non-irradiated fish.

• 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.

• 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.12 no.4
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• pp.477-480
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• 2003

Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organochlorine and pyrethroid pesticides using GC(ECD). An ultra-2 fused silica capillary column was used to separate and identify the products. The resolution between the last isomeric peak of cypermethrin(59.987min) and the first isomeric peak of flucythrinate(60.043min) was not satisfactory. The last isomeric peak of fenvalerate(62.344min) and the first isomeric peak of fluvalinate(62.397min) were overlapped. Recoveries of soybean sample fer the most pesticides were 73.3% to 102.4%. Detection limits were between 0.004 and 0.063 ${\mu}$g/mg when this method was used.

• Journal of Applied Biological Chemistry
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• v.43 no.2
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• pp.94-100
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• 2000

An analytical method was developed to determine abamectin and milbemectin residues in apple, pear, and citrus using HPLC with ultraviolet absorption detection. Abamectin and milbemectin were extracted with methanol from apple, pear, and citrus samples. The extract was diluted with saline water and dichloromethane partition was followed to recover the compounds from the aqueous phase. Florisil column chromatography and aminopropyl solid-phase extraction were employed as cleanup methods to remove most of co-extractives from the sample extract. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate abamectin and milbemectin residues in sample extracts at the wavelength of 245 nm. Recoveries of abamectin and milbemectin from fortified samples ranged 80.4~90.3% and 90.9~96.8%, respectively. Relative standard deviations of the analytical method were less than 10% for both acaricides. Detection limit of the analytical method was 0.003 mg/kg sample for all the analytes. The proposed method was reproducible and sensitive enough to evaluate terminal residues of abamectin and milbemectin in apple, pear, and citrus.

• Journal of Applied Biological Chemistry
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• v.42 no.4
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• pp.191-196
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• 1999

A multiresidue analytical method was developed for eight acaricides including benzoximate, clofentezine, fenazaquin, fenothiocarb, fenpyroximate, hexythiazox, pyridaben, and tebufenpyrad in four major fruits using high-performance liquid chromatography (HPLC). All the confounds were extracted with acetone from apple, pear, grape, and citrus samples. The extract was diluted with saline water, and n-heaxane partition was followed to recover the acaricides. Florisil column chromatography was employed to further purify the sample extract. HPLC with ultraviolet absorption detection, using an octadecylsilyl column under the isocratic mobile phase of acetonitrile/water mixture, was successfully applied to separate and quantitate all the compounds in the purified extract. Recoveries of the eight acaricides from for fortified samples ranged 86.4~97.0%. Relative standard deviations of the analytical method were all less than 10%. Detection limits of the method were in the range of 0.02~0.05 mg/kg. The proposed method was reproducible and sensitive enough to evaluate the terminal residue of the eight acaricides in the fruit harvest.

• Analytical Science and Technology
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• v.15 no.5
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• pp.466-474
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• 2002

The analytical method of 14 kinds of coplanar - PCBs was established and applied the soil sample. The three kinds of extraction solvents (toluene, acetone: n-hexane, dichloromethane) were selected to apply the soil sample. The silica gel, florisil and alumina column cleanup also performed to compare the elution recovery. The average recovery of selected solvents in soil A, B and C was surveyed the 84.25%, 56.09% and 44.69% for toluene, 52.56%, 81.42% and 58.53% for acetone : n - hexane and 55.94%, 71.33% and 61.05% for dichloromethane. The average recovery is represented 49.99% for silica gel (n - hexane 100 mL), 69.65% for florisil (6% ether/n - hexane 100 mL), and 65.23% for alumina (2% DCM : n - hexane 100 mL, 50% DCM: n-hexane 150 mL). In silica gel (n - hexane) and florisil (6% ether : n - hexane) cleanup, the 14 kinds of coplanar PCBs eluted until 40 mL. In the silica gel and florisil columns cleanup, the amounts of elution solvent can be reduced from these results, but the researcher has to confirm the elution amounts before performing the experiments. In alumina cleanup process, the result was obtained to the 100 mL of elution solvents (2% DCM: n-hexane 100 mL and 50% DCM: n-hexane 40 mL), therefore the change of elution solvent is necessary to develop the simple procedure.

• Korean Journal of Food Science and Technology
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• v.40 no.2
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• pp.123-128
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• 2008

The MRLs (maximum residue limits) of DDT (DDD and DDE) in fresh ginseng, dried ginseng, and steamed red ginseng are set as low as 0.01 mg/kg, 0.05 mg/kg, and 0.05 mg/kg, respectively. Therefore, this study was undertaken to develop a simple and highly sensitive analysis method, as well as to reduce interfering ginseng matrix peaks, for the determination of DDT isomers (o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in fresh ginseng, dried ginseng, and steamed red ginseng at the 0.01 mg/kg level. The method used acetonitrile extraction according to simultaneous analysis, followed by normal-phase Florisil solid-phase extraction column clean-up. The purification method entailed the following steps: (1) dissolve the concentrated sample extract in 7 mL hexane; (2) add 3 mL of $H_2SO_4$; (3) vigorously shake on avortex mixer; (4) cetrifuge at 2000 rpm for 5 min; (5) transfer 3.5 mL of the supernatant to the Florisil-SPE (500 mg/6 mL);and (6) elute the SPE column with 1.5 mL of hexane and 10 mL of ether/hexane (6:94). The determination of DDT isomers was carried out by a gas chromatography-electron capture detector (GC-${\mu}$ECD). The hexane and ether/hexane (6:94) eluate significantly removed chromatographic interferences, and the addition of 30% $H_2SO_4$ to the acetonitrile extract effectively reduced many interfering ginseng matrix peaks, to allow for the determination of the DDT isomers at the 0.01 mg/kg level. The recoveries of the 6 fortified (most at 0.01 mg/kg) DDT isomers from fresh ginseng, dried ginseng, and steamed red ginseng ranged from 87.9 to 99.6%. The MDLs (method detection limits) ranged from 0.003 to 0.009 mg/kg. Finally, the application of this method for the determination of DDT isomers is sensitive, rapid, simple, and inexpensive.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.345-353
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• 2015

The aim of this study is to develop residue analysis method for fenoxanil, a MBI (melanin biosynthesis inhibitor) propionamide fungicide, had mainly been used to control rice blast, and disease of other crops, fruits, and vegetables by using GLC/NPD and GC/MS. Extraction with acetone and partition with n-hexane/dichloromethane (80/20, v/v) were performed from hulled rice, soybean, Kimchi cabbage, green pepper, and apple, then column clean-up with florisil was applied. Mean recoveries were 82.2%-109.1% with less than 7.2% of coefficients of variation and limit of quantitation was set at the concentration of 0.04 mg/kg from the five agricultural products through the determination by GLC/NPD equipped with DB-5 capillary column and single laboratory validation. As a confirmatory method, GC/MS selected ion monitoring (SIM) was set from m/z 125.0, 188.9, and 293.0. Developed method is expected to apply the single residue analysis of fenoxanil in agricultural products.