• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.57-65
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• 2018

BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

• The Korean Journal of Pesticide Science
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• v.14 no.1
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• pp.37-48
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• 2010

The diacylhydrazine insecticides, methoxyfenozide, chromafenozide and tebufenozide are new-generation insecticides. These insecticides induce premature molting and cause the death of insects by mimicking their hormone. Also, these insecticides have already been widely used for vegetables planting in worldwide. Highperformance liquid chromatography (HPLC) is the most widely used procedure for determination of each compound residues in crops. However, simultaneous analysis method of these diacylhydrazine insecticides was not reported. The purpose of this study is to develop a simultaneous determination procedure of methoxyfenozide, chromafenozide and tebufenozide residue in crops using HPLC-UVD/MS method. These insecticide residues were extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were quantitated by HPLCUVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at two levels per crop. Mean recoveries ranged from 89.0 to 104.8% in five representative agricultural commodities. The coefficients of variation were less than 3.9%. Quantitative limits of methoxyfenozide, chromafenozide and tebufenozide were 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of methoxyfenozide, chromafenozide and tebufenozide in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.360-365
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• 2007

The studies for the derivatization of 3-monochloropropane-1,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PBA (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-[tert.-butyldimethylsilyl] trifluoroacetamide) and acylation with MBTFA (N-Methyl-bis[trifluoro-acetamide]) were also considered. Except the TBDMS derivative of 3-MCPD, all the derivatives were detected well. The derivatives of 3-MCPD with HFBI, PBA and BSTFA showed below 10 ${\mu}g/kg$ which was sensitive enough to satisfy Korea maximum residue limit 0.3 mg/kg. Among the tested adsorbents, Extrelut20 and Florisil were evaluated as the proper adsorbents to eliminate the soy sauce matrix for 3-MCPD. Ethyl acetate was the most efficient eluent with good recovery rate. The desired surrogate compound and internal standard were 1,2-butanediol and 1,2-dibromo-3-chloropropane, respectively. The limit of detection for PB-MCPD and TMS-MCPD were 10.16 and 7.06 ${\mu}g/kg$ on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 ${\mu}g/kg$ by GC/ECD and GC/MSD, respectively.

• Korean Journal of Food Science and Technology
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• v.30 no.5
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• pp.1018-1023
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• 1998

Hydrocarbons in dry soup base and its ingredients in instant noodle were analyzed to determine whether the analysis of hydrocarbons is a potential method to detect post-irradiation of the soup base. Soup base ingredients were irradiated individually, irradiated before mixing, or mixed after irradiation. Lipids were extracted with hexane and hydrocarbons were separated from the lipids through Florisil column. The hydrocarbons were analyzed with GC. Hydrocarbons C17:2, C16:3, C17:1, and C16:2 were detected in palm oil, red pepper powder, and sesame seeds irradiated at 10 kGy, but not in unirradiated ones. C17:2, C16:3, C17:1, and C16:2 were not detected in the soup base mixture of unirradiated ingredients. The four hydrocarbons were detected in the soup base mixture using irradiated palm oil or sesame seeds. In the mixture using irradiated red pepper powder, C17:2 and C16:3 were detected. When the soup mixture was irradiated after mixing unirradiated ingredients, C17:2, C17:1, and C16:2 were detected in the sample irradiated at 1 kGy, and C17:2, C16:3, C17:1, and C16:2 were in large amounts at 5 and 10 kGy.

• Korean Journal of Environmental Agriculture
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• v.21 no.2
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• pp.90-95
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• 2002

A study was carried out to optimize the cleanup step using a solid-phase extraction (SPE) cartridge, $SupelClean^{TM}$ Florisil, for multiresidue analysis of 16 pesticides in cucumber matrix. Eluting efficiencies of two solvent systems including acetone/n-hexane and ethyl acetate/n-hexane mixtures were critically evaluated by recoveries of target anaytes from the SPE Florisil column. Based on the recovery as a measure of eluting efficiency, an acetone/n-hexane (20/80,v/v) mixture provided more than 80% recovery for 15 pesticides except bifenthrin. In case of ethyl acetate/n-hexane, 14 pesticides showed recoveries higher than 75% while those far alachlor and bifenthrin were less than 30%.

• Korean Journal of Food Science and Technology
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• v.41 no.2
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• pp.157-161
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• 2009

This paper proposes an analytical method for determining amounts of polycyclic aromatic hydrocarbons (PAHs; benzo[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenzo[a,h]anthracene, benzo[g,h,i] perylene) in coffees beans. Soxhlet extraction and liquid/liquid extraction were tested for the quantification of seven PAHs. Soxhlet extraction was followed by cyclohexane extraction and used a silica cartridge. Liquid/liquid extraction was followed by n-hexane extraction and utilized a florisil cartridge. The extracts were analyzed by HPLC-fluorescence detection (FLD) with a Supelcosil LC-PAH column. The PAH recoveries ranged from 78.68 to 96.28% for the liquid/liquid extraction, and from 67.47 to 84.60% for the Soxhlet extraction.

• Analytical Science and Technology
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• v.23 no.2
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• pp.196-204
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• 2010

In this study, the following concentrations of some PAHs (Polycyclic Aromatic Hydrocarbons) were investigated; [benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene] in processed foods (n=165) and cooked meats (n=45) and established the analytical method by characteristics of processed foods. The methodology involved extraction (alkali digestion, liquid-liquid extraction, microwave extraction), clean-up on Sep-Pak Florisil Cartridges and determination by HPLC/FLD (High Performance Liquid Chromatography/Fluorescence Detector). The recovery of overall method for 8 PAHs spiked into these products ranged from 92 to 103%. The mean level of detected foods was found to be benzo(b)fluoranthene $0.9\;{\mu}g/kg$ in smoked salmon, benzo(b)fluoranthene $1.0\;{\mu}g/kg$, benzo(k)fluoranthene $0.3\;{\mu}g/kg$, benzo(a)pyrene $0.9\;{\mu}g/kg$ in dried banana, benzo(b)fluoranthene $0.2\;{\mu}g/kg$, benzo(k)fluoranthene $0.1\;{\mu}g/kg$, benzo(a)pyrene $0.2\;{\mu}g/kg$ in smoked chicken, benzo(b)fluoranthene $1.3\;{\mu}g/kg$, benzo(k)fluoranthene $0.3\;{\mu}g/kg$, benzo(a)pyrene $0.9\;{\mu}g/kg$ in charcoal grilled pork, respectively.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.309-317
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• 2015

BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.37 no.6
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• pp.866-872
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• 2005

Cocentrations of PAHs [benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h.i)perylene, indeno(1,2,3-c,d)pyrene] in fish (n=120), shellfish(n=50) and their products (n=35) were estimated by saponification and extraction with n-hexane, clean-up on Sep-Pak Florisil Cartridges and HPLC/FLD. Overall recoveries for eight PAHs spiked into samples ranged from 90 to 106%. Mean level of benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene and indeno(1,2,3-c,d)pyrene were not detected, 0.01, 0.04, 0.07, 0.05, 0.004, 0.0008 and 0.06ng/g, respectively, similar to those reported by other countries.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.389-400
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• 2011

A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.