GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및Trifluralin의 동시 분석
Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS
2
조회
0
다운로드
1
인용
0
참고문헌
키워드
초록
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.
Abstract
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.
참고문헌 (22)
- 안경근, "HPLC-UVD", MS를 이용한 농산물 중 Amisulbrom의 잔류분석, 2014, pp.18(4), 321~329[DOI]
- Canadian Council of Ministers of the Environment, "Canadian water quality guidelines for the protection of aquatic life, metolachlor", pp.1~3 (1999), Manitoba Statutory Publications
- Dharumarajan, S., "Persistence of pretilachlor in coastal rice ecosystem", Pesticide Research Journal, 20(2), pp.273~274 (2008)
- Fong, W. G., "Pesticide residues in food: methods. Technologies, and Regulations", pp.3~44 (1999), Wiley Interscience
- Hutson, D. H., "Metabolic pathways of agrochemicals, herbicides and plant growth regulators", pp.216~217 (1998)
- Judge, C. A., "Trifluralin (Preen) dissipation from the surface layer of a soilless plant growth substrate", Journal of Environmental Horticulture, 21(4), pp.216~222 (2003)
- Jursik, M., "Efficacy and selectivity of post-emergent application of flumioxazin and oxyfluorfen in sunflower", Plant Soil Environment, 57(11), pp.532~539 (2011)[DOI]
- 김미옥, "LC", MS, 한국식품과학회지, pp.2010, 42(6)[DOI]
- Kwon, C. H., "Terminal residues of monocrotophos and phosphamidon in apples", Life Science Research, 1(3), pp.277~286 (2003)
- 이종화, "시설 내 오이 재배 중 살균제 Boscalid의 잔류특성", 농약과학회지, 12(1), pp.67~73 (2008), 한국농약과학회
- Barefoot, A., "Handbook of residue analytical methods for agrochemicals (Vol. 2)", pp.585~ (2003), Wiley
- 이수진, "HPLC-UVD", MS를 이용한 농산물 중 ametryn의 분석, 2011, pp.15(2), 125~133[DOI]
- MS, "Identification of trifluralin metabolites in soil using ion-trap LC", MS
- Li, H. P., "Fast multi-residue screening for 84 pesticides in tea by gas chromatography with dual-tower auto-sampler, dualcolumn and dual detectors", Journal of the Chinese Chemical Society, 51(3), pp.531~542 (2004)[DOI]
- Mastovska, K., "Pesticide multiresidue analysis in cereal grains using modified QuEChERS method combined with automated direct sample introduction GC-TOFMS and UPLC-MS", MS techniques, 2010, pp.58(10), 5959~5972
- Miller, J. M., "Chromatography : Concepts and contrasts, standardization administration of the people's republic, (2nd)", pp.286~287 (2005), Wiley Intersciense
- Park, C. J., "Persistence of the fungicide boscalid in grapes and strawberries", Life Science Research, 2(2), pp.9~16 (2003)
- Raina, R., "Comparison of gas chromatography -mass spectrometry and gas chromatography-tandem mass spectrometry with electron ionization and negative-ion chemical ionization for analyses of pesticides at trace levels in atmospheric samples", Analytical chemistry insights, 3, pp.111~125 (2008)
- Shackelford, D. D., "Determination of ethalfluralin in canola seed, meal, and refined oil by capillary gas chromatography with mass selective detection", Journal of agricultural and food chemistry, 48(9), pp.4422~4427 (2000)[DOI]
- The Dow Chemical Company, "Product safety assessment for ethalfluralin", pp.1~6 (2010)
- Yokley, R. A., "Analytical method for the determination of metolachlor, acetochlor, alachlor, dimethenamid, and their corresponding ethanesulfonic and oxanillic acid degradates in water using SPE and LC", ESI-MS, Analytical chemistry, pp.2002, 74(15)[DOI]
- Yun, H. C., "Monitoring the residual pesticide levels of soil and water from the main agricultural area in Busan (II)", The Annual Report of Busan Metropolitan City Institute of Heath & Environment, 19(1), pp.72~80 (2009)