• Horticultural Science & Technology
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• v.34 no.1
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• pp.183-194
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• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 1997.10a
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• pp.37-39
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• 1997

Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

• Korean Journal of Pharmacognosy
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• v.12 no.4
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• pp.211-214
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• 1981

Solanesol has been isolated from aged Korean native tobacco leaf(Hyangcho and Sohyang) by water pretreatment, hexane extraction and column chromatography on Florisil in yields of 0.41% and 0.31% dry wt., respectively. Thin-layer densitometric analysis of the hexane extracts of samples(Hyangcho Sohyang) has shown that the amounts of solanesol present are 0.74% and 0.52% dry wt., respectively.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.185-194
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• 2015

This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

• Journal of the Korean Chemical Society
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• v.29 no.5
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• pp.496-502
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• 1985

The solvent extraction and cleanup processes for the simultaneous gas-liquid cliromatographic determination of 16 kinds of organochlorine pesticide residues were investigated. The pesticides were extracted out from-various crops with the aqueous acetone solution acidified (pH < 1.5) by adding conc. $H_3PO_4$. Most of the pesticides were partitioned from the solution with petroleum ether. Evaporated the extracting solvent, the residues were dissolved in ethylether-petroleum ether (6 : 94) eluent and eluted through the Florisil column activated at 650$^{\circ}$C for 2.5hrs. The extraction efficiency was over 94% and impurities were effectively removed by the column chromatography.

• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.117-124
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• 2018

BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

• Journal of the Korea Convergence Society
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• v.9 no.4
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• pp.75-84
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• 2018

This study investigated the pollution status of polycyclic aromatic hydrocarbons (PAHs) such as benzopyran, which is a harmful substance, in convergence herbal pills distributed in Seoul. During 2010 ~ 2013, 31 items and 93 samples were collected from the herbal medicines vendors in Seoul, and the samples were extracted, filtered, concentrated, and then spun out with SPE (Sep-pak florisil) and concentrated again and analyzed by liquid chromatography. The results of the analysis showed that the average contents of PAHs were below $10{\mu}g/kg$, and the PAHs were lower than those of daily life exposure, and MOEs was evaluated as safe to a negligible level. In the future, comparative fusion studies on the harmful substances of medicinal pills and food pills are needed.

• Analytical Science and Technology
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• v.9 no.2
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• pp.123-133
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• 1996

The optimum conditions for the analysis of the difenoconazole fungicide on soil and crops were investigated and the residues of that in apple and soil were identified by using the gas chromatography. The extract with acetonitrile was separated with saturated NaCl and n-hexane solution after filtered, and concentrated. Obtained fungicide residues were transfered to the florisil column and eluted with acetone and n-hexane mixed solution for the analysis by GLC(ECD). From the standard addition experiments with 0.20 and 1.0ppm, the average recoveries were 86~92% and the detection limit was 0.01 ppm. It seems to be safely used when difenoconazole is treated three times until 15 days before harvest of apple. In this case residual amounts of difenoconazole in apple was from 0.037ppm to 0.044ppm. The soil samples extracted with methanol and ammonium hydroxide mixed solution were partitioned with dichloromethane and saturated sodium chloride solution. The organic phase was concentrated and redissolved with toluene and analyzed with GLC(FID) after cleaned with Sep-Pak column. From the standard addition experiments with 0.10, 0.50 and 1.0ppm, the average recoveries were 101.2~103.7% and the detection limit was 0.025ppm.

• Journal of the Korean Society of Food Science and Nutrition
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• v.33 no.1
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• pp.158-163
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• 2004

We investigated the usefulness of 2-alkylcyclobutanones as markers for irradiated eggs and egg products by comparing 2-alkylcyclobutanone concentrations in irradiated raw egg yolk, boiled egg yolk, and egg yolk powder. One method of detection radiation-induced 2-alkylcyclobutanones involves extraction fat from irradiated egg samples separating 2-alkylcyclobutanones by florisil column chromatography, and identifying GC/MS. 2-(5'-Tetradecenyl)cyclobutanone of 2-alkylcyclobutanones was high relatively in boiled egg yolk, but 2-dodecylcyclobutanone was high in raw egg yolk and egg yolk Powder. Concentrations of the radiation-induced 2-alkylcyclobutanones increased linearly with the irradiation dose. The radiation-induced 2-alkylcyclobutanones from egg samples at 0.5 kGy over and not detected at the non-irradiated samples. Therefore, these compounds could be used as marker of Post-irradiation for egg Products.

• 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.