• 대한예방의학회:학술대회논문집
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• 2005.10a
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• pp.388-388
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• 2005

• Korean Journal of Environmental Agriculture
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• v.28 no.4
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• pp.427-434
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• 2009

Analytical method for prochloraz in cabbage, apple, pepper, mandarin, and hulled rice was established by conversion it to 2,4,6-trichlorophenol (TCP). Crop samples were extracted with acetonitrile, and partitioned with dichloromethane. The sample extracts were hydrolyzed with pyridine hydrochloride in a vial by heating for 1 hour, and analyzed with GC-ECD after partitioning with dichloromethane. Method quantification limit (MQL) of prochloraz was 0.01 mg/kg. Recoveries at 0.1 mg/kg level was 105-113% while at 0.5 mg/kg level was 82-87%. In both of the cases CV was less than 10%. Through this procedure soxhlet extraction and refluxing apparatus of conventional method were discarded and simple solvent extraction and small vial were successfully employed, resulting in simple, rapid, economic and more precise method.

• Analytical Science and Technology
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• v.10 no.3
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• pp.168-178
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• 1997

The optimum conditions for the residual analysis of the ethalfluralin herbicide on soils were investigated and the residues in soils were determined by gas chromatography with electron capture detector(GC-ECD). The soil samples extracted with methanol and dichloromethane and concentrated. The concentrated phase were redissolved with toluene and analyzed with GC-ECD after separated by cyanosilica gel Sep-Pak cartridge. From the standard addition experiments with 0.1 and 1.0ppm, the average recoveries were 92.8~101.2% and the detection limit was 0.004ppm. The half-life time of ethalfluralin in the soil(A) was 35 days in the laboratory and 7.2 days in the field test whereas it was 45 days and 9.7 days for each in case of soil(B).

• The Korea Journal of Herbology
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• v.21 no.4
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• pp.37-41
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• 2006

Objectives : This study has been conducted to investigate the amount of residual pesticide in herbal medicine of Osterici Radix which are purchased on Kwangju(Hanyaksarang). Methods : In order to analyze many pesticides in Osterici Radix, simultaneous multi-residue analysis of pesticides by GC-ECD/NFD was used. Results : But the amount of residual pesticide in Osterici Radix, simultaneous multi-residue analysis of pesticides by GC-ECD/NFD was used. Conclusion : These results indicate that Osterici Radix in current has safety. In future, it is considered the results of this study will be furnished the basis to succeeding studies and it is needed to extensive comparative study for the same genus-degree of relatedness.

• Journal of Food Hygiene and Safety
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• v.27 no.4
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• pp.332-338
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• 2012

A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.

• Journal of Food Hygiene and Safety
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• v.12 no.4
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• pp.288-293
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• 1997

Analytical method using capillary GC/ECD was developed to determine trace residues of chlofluazuron, 1-[3, 5-dichloro-5-trifluoromethyl-2-pyridyloxy)phenyl]-3-(2, 6-difiuorobenzoyl), in meat, and applied to analyze the residues in domestic and imported meats. The analytical scheme developed does not require column chromatographic cleanup; chlorfiuazuron was extracted with diethyl ether and petroleum ether (50: 50), partitioned against acetonitrile, cleaned up with silica Sep-Pak cartridge, identified GC/ECD, and comfirmed by GC/MS. The mean recoveries of the pesticide in meat fortified with standard solution 0.1, 0.5, 0.1 mg/kg were ranged from 82 to 95%. The limit of detection and limit of quantitation were 0.001 and 0.005 mg/kg, respectively. Chlorfluazuron residues were not found in domestic samples, but found in imported Australian beef ranging from 0.02 to 0.17 mg/kg, detected by 18% among the samples.

• Archives of Pharmacal Research
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• v.15 no.2
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• pp.109-114
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• 1992

For the risk assessment of human exposure to volatile halogenated hydrocarbons, a dynamic purge trap/on-column cryofocusing method using capillary gas chromatograph-$^{63}Ni$ electron capture detector and thermal desorption unit was applied to analyze the free forms, metabolites of 1, 1, 2-trichloroethylene and 1, 1, 2, 2-tetrachloroethylene. The urine sample was diluted with distilled water, hydrolyzed and sealed. Then the inert gas was infused to purge out free 1, 1, 2-trichloroethylene, free 1, 1, 2, 2-tetrachloroethylene and urichloroethanol. These compounds were trapped to $Tenax^R$ / GC-gas trap device throughout clean up tube. Being undertectable to gas chromatograph directly, trichloroacetic acid was methyl esterificated and trapped in the manner above mentioned. The optimal incubation time to get best recovery of methyl ester was 4 hours at $60^circ$C. The concentrations of free volatile halogenated hydrocarbons and their metabolites in urine were obtained of free volatile halogenated hydrocarbons and their metabolites in urine were obtained from 5 healthy volunteers. This analytical method is expected to make the biological monitoring more precise and convenient.

• Journal of Applied Biological Chemistry
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• v.63 no.2
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• pp.153-159
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• 2020

The analytical method was established for simultaneous determination of fungicide prochloraz and its metabolites in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). Samples including beef meat, pork meat, chicken meat, milk, and egg were hydrolyzed with pyridine hydrochloride which converts prochloraz and its metabolites to 2,4,6-trichlorophenol (2,4,6-TCP) because residue definition for prochloraz was 'sum of prochloraz and its metabolites containing the 2,4,6-trichlorophenol moiety, expressed as prochloraz', for compliance with MRLs from animal commodities. Therefore, residual prochloraz was extracted with acetone, decomposed to 2,4,6-TCP, partitioned with dichloromethane, purified with aminopropyl SPE and quantified as 2,4,6-TCP with GC-ECD. The instrumental limit of quantitation and method LOQ (MLOQ) was 0.01 ㎍/mL and 0.02 mg/kg for prochloraz and 0.005 ㎍/mL and 0.01 mg/kg for 2,4,6-TCP, respectively. The linearity of the calibration curve was good with R² >0.995 in the range of 0.005-0.2 ㎍/mL. Fortification levels of prochloraz were 0.02 mg/kg (MLOQ) and 0.2 mg/kg (10MLOQ) for recovery tests. Overall recoveries of prochloraz were >90% with <10% of coefficient variation (C.V.). This established analytical method was fully validated and could be useful for quantification of prochloraz and its metabolites in animal commodities as official analytical method.

• Korean Journal of Food Science and Technology
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• v.46 no.1
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• pp.7-12
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• 2014

A sensitive and simple analytical method to identify flutianil residues in agricultural commodities was developed and validated using gas chromatography-electron capture detection (GC-ECD) and mass spectrometry (GC-MS). The flutianil residues were extracted with acetonitrile, partitioned with dichloromethane, and then purified using a silica solid-phase extraction (SPE) cartridge. The method was validated using pepper, sweet pepper, mandarin, hulled rice, soybean, and potato spiked with 0.02 or 0.2 mg/kg flutianil. The average recovery of flutianil was 76.5-108.0% with a relative standard deviation of less than 10%. The limit of detection and limit of quantification were 0.004 and 0.02 mg/kg, respectively. The result of recoveries and relative standard deviation were in line with Codex Alimentarius Commission Guidelines (CAC/GL 40). These results show that the method developed in this study is appropriate for flutianil identification and can be used to maintain the safety of agricultural products containing flutianil residues.

• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.104-116
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• 2018

BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were 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 saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) 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. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% 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 the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) 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 residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.