The Determination Methods Of Fenpyroximate Residues In Honey And Royal Jelly

The objective of this paper was researching a new method for detection,confirmation and quantification of fenpyroximate and its isomer residues in honey and royal jelly.Methods were developed and validated for the determination of fenpyroximate in honey by Ultra performance liquid chromatography(UPLC)and in honey and royal jelly by liquid chromatography-tandem mass spectrometry(LC-MS/MS),respectively.Methods for the determination of fenpyroximate in fruits and vegetables have been in successfully reported.However,research papers concerning the determination of fenpyroximate in honey and royal jelly are very limited.The results of this work fill the blank of the the standards for the agro-products in our country and provide a scientific basis for the validation of the export honey.1.A simple and rapid method of determination of fenpyroximate residue in honey by UPLC was developed.The analytes was extracted,and cleaned-up by solid-phase extraction step.The chromatographic separation of analytes was performed on a BEH C1 8(2.1×50mm,1.7μm Waters)reversed-phase column using an acetone-water(70:30,v/v)as flow rate 0.2mL/min,injection volume is 2μL,the column temperature was set on 40℃,and set ultraviolet detection at 258nm wavelength.The(E)-fenpyroximate and(Z)-fenpyroximate chromatographic behavior is good through optimizing the separation conditions,the retention time were 2.4 min and 3.2 min.The linear ranges was from0.01～0.5 mg/L and the correlation coefficients(r~2)were all greater than 0.999.The recoveries for(E)-fenpyroximate and(Z)-fenpyroximate at three spiked levels(0.05、0.1、0.2mg/kg)were in the range of 98.6～103.9%and97.4～103.4%with relative standard deviations(RSDs,n=5)of 0.51～2.0%and 1.5～3.7%,the respective limits of detection was4.2μg/kg and 4.3μg/kg.Employment and suitability test measured(E)-fenpyroximate and(Z)-fenpyroximate add concentrations at 0.05,0.1,0.2 mg/kg respectively the average recovery between 99.8%～103.0%and 97.4%～101.4%,RSD between 0.31%～3.9%and 0.74%～4.7%respectively.2.An analytical method for the determination of fenpyroximate residue by LC-MS/MS in honey was developed.In the procedure the samples were extracted and purificated,then separated by liquid chromatographic and tandem mass spectrometry analysis.Mass spectral acquisition was applied with multiple reaction monitoring of two diagnostic transition reactions.The qualitative analysis was based on the retention time,the precursor ion and two productions,and the quantitation was carried out with intension of the characteristic ion m/z366.The linear ranges were from0.1～100μg/L for fenpyroximate and the correlation coefficients(r~2)were all greater than 0.999.The average recoveries for fenpyroximate ranged was 85.8%～113.2%with relative standard deviations(RSDs,n=5)of 1.2-4.3%,the detection limits was O.01μg/kg,the fenpyroximate residues were detected in two honey samples among 20 samples.3.A high performance liquid chromatography tandem mass spectrometric(HPLC-MS/MS)method was developed for the determination of fenpyroximate in royal jelly.Select the optimal extracting solution,solid phase extraction column and the elution by orthogonal experiment.The linear range was from5～100μg/L for fenpyroximate and the correlation coefficients(r~2)were all greater than 0.999.In replicate sets of royal jelly samples spiked with the drug concentration of 5,10,and50μg/kg,the average recoveries for fenpyroximate ranged were 88.5%～96.6%with relative standard deviations(RSDs,n=5)of 4.5-8.1%,and the relative standard deviations(RSDs)were less than 10.8%for intra-day and 10.3%for inter-day determinations.The detection limits was 0.1μg/kg.The dietary exposure assessment result of fenpyroximate in royal jelly show that the risk of acute dietary exposure value(%ARfD)and chronic dietary risk value(%ADI)were less than 100.The man and woman acute dietary exposure value(%ARfD)were 0.0072～0.0356 and 0.0058～0.0395,respectively.The man and woman chronic dietary risk value(%ADI)were 0.0030～0.0150 and 0.00240.0167,respectively.As the growth of the age,the risk of%ARfD and%ADI are higher and higher.