Rapid and sensitive determination of two degradation products of flumethrin in honey by ultrasonically assisted extraction and gas chromatography with electron capture detection.
A rapid and sensitive method for the determination of 4-fluoro-3-phenoxybenzaldehyde cyanohydrin (FPBC) and 4-fluoro-3-phenoxy-benzaldehyde (FPB) in honey samples using ultrasonically assisted extraction and gas chromatography with electron capture detection (GC-ECD) has been developed. The different factors affecting the efficiency of the extraction were carefully optimized. The honey sample was extracted with a mixture of hexane and dichloromethane (v/v, 1:1) utilizing the ultrasonically assisted technique and cleaned up by solid-phase extraction on Oasis HLB cartridges. The eluate was evaporated to dryness and residues were reconstituted to 1.0 mL with hexane and determined by GC-ECD. The calibration curves of fortified samples showed acceptable linear response (R(2) >0.99) over a range of 3-100 ng/g for FPBC and FPB in seven replicate determinations of six concentrations, respectively, and analysis of variance (ANOVA) with a lack-of-fit test was performed to validate the regression data. Overall average recoveries ranged from 90.9 to 106.2% for honey samples. The detection limits were 0.9 ng/g for FPBC and 1.0 ng/g for FPB, respectively. This method can be successfully applied to routine determination of two degradation products of flumethrin in honey samples.
Zhou
Jinhui
J
Bee-product Quality Supervision and Testing Center, Ministry of Agriculture, Apicultural Research Institute, Chinese Academy of Agricultural Sciences, Beijing, PRC.
Xue
Xiaofeng
X
Li
Yi
Y
Zhang
Jinzhen
J
Wu
Liming
L
Chen
Lanzhen
L
Zhao
Jing
J
D000096:Acetone / Q000032:analysis; D001547:Benzaldehydes / Q000737:chemistry*; D002623:Chemistry Techniques, Analytical / Q000379:methods; D002849:Chromatography, Gas / Q000379:methods*; D004583:Electrons; D006586:Hexanes / Q000032:analysis; D006722:Honey; D008752:Methylene Chloride / Q000032:analysis; D008956:Models, Chemical; D009570:Nitriles / Q000737:chemistry*; D010936:Plant Extracts / Q000737:chemistry; D011722:Pyrethrins / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents
D001547:Benzaldehydes; D006586:Hexanes; D009570:Nitriles; D010936:Plant Extracts; D011722:Pyrethrins; D012997:Solvents; C430593:cyanohydrin; D000096:Acetone; C041392:flumethrin; D008752:Methylene Chloride