Study On The Determination Of Pesticide Residues In Wine And Honey By SPME

In recent years,the consumptions of wine and honey have been showing a rapid growth trend.Grapes as a raw material for wine,in the planting and production processes will be sprayed a large number of pesticides,including herbicides,fungicides,insectifuges and so on.Although in the production and fermentation processes,some of the pesticides will dilute or degrade,there are still some pesticide residues in wine.Amitraz as an acaricide is used to combat honeybee's diseases.However,amitraz and its metabolites 2,4-dimethylaniline(DMA)are toxic and carcinogenic.Pesticide residues will be accumulated in the human body in long-term,and will endanger human health.In this paper,pesticide residues in wine and honey are investigated.Solid-phase microextraction(SPME)and gas chromatography tandem mass spectrometry(GC-MS/MS)were employed as pretreatment and detection method in this study.161 kinds of pesticide residues in wine,and amitraz and DMA in honey were qualitatively and quantitatively analyzed.(1)Gas chromatography/tandem mass spectrometry was established to determine 161 pesticides.DB-1701 column was used and the rising temperature program was optimized to complete separate 161 compounds.(2)SPME pretreatment method for determination of the pesticide residues in wine was established.The 85 ?m-PA fiber was employed to extract the analytes after considering the factors of the number of extracting target compounds,the stability of the extraction fiber,and the residues of the extraction fiber.The pretreatment conditions,including the amount of sample,extraction temperature,stirring speed,extraction time,ionic strength,pH and etc.were optimized.(3)The proposed method was evaluated according to detection limits,linearity,recovery rate and precision.The results showed the proposed method can detect 101 target pesticides in the same time,and the linear correlation coefficient was more than 0.99 for most pesticides.The quantitation limits were below 10 ?g/L for 90% of the pesticides.Single sample analysis time was less than 1 hour with this method,and more than 100 pesticide residues could be determined simultaneously in a single sampling.(4)Simultaneous determination of amitraz and its metabolite 2,4-dimethylaniline(DMA)in honey by SPME/GC-MS/MS was developed.The highest response value of amitraz and DMA could be obtained when samples were extracted at room temperature for 45 min at a stirring speed of 750 rpm using the 85 ?m-PA fiber at the optimized conditions,the limits of detection for amitraz and DMA were 0.5 ?g/kg and 3.0 ?g/kg,respectively.The spiked recoveries of amitraz and DMA were 81.9%-98.2% and 75.5%-90.6% respectively.The relative standard deviations(RSDs)of amitraz and DMA were 5.0%-15.4% and 7.9%-17.2% respectively.