The Determination Methods Of Multi-acaricide Residues In Honey And Royal Jelly

The objective of this paper was researching a new method for detection, confirmation and quantification of 10 acaricides residues in honey and royal jelly. Methods were developed and validated for the determination of 10 acaricides in honey and royal jelly by liquid chromatography-tandem mass spectrometry(LC-MS/MS), respectively. Methods for the multi-residue of pesticides and the determination of antibiotics have been successfully reported. However, research papers concerning the determination of acaricides 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 rapid high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method has been developed for the determination of ten acaricides(Clofentezine, Fenazaquin, Tebufenpyrad, Hexythiazox, Etoxazole, Coumaphos, Pridaben, Propargite, Spirodiclofen, Fenpyroximate) in honey with ultrasonic-assistant dispersive liquid-liquid microextraction(DLLME). The qualitative and quantitative analysis for the analytes were carried out under the multi-reaction monitoring(MRM) mode with positive mode in matrix-matched standard method. Under the optimal conditions, the calibration curves were linear in the range of 0.1-100 μg/L for 10 acaricides. The limites of quantitation(LOQs) were 3.0 μg/kg for clofentezine, fenazaquin, hexythiazox, etoxazole and spirodiclofen, 1.5 μg/kg for coumaphos, pridaben and propargite, 2.0 μg/kg for tebufenpyrad, and 2.5 μg/kg for fenpyroximate. The blank honey sample spiked in three concentrations at 10、50、100 μg/kg, the recoveries ranged from 72% to 107%, with the ralative standard deviations less than 12%. Among the determination of 100 honey samples, the determinative rate were 9% for Clofentezine, 5% for Fenazaquin, 16% for Tebufenpyrad, 12% for Hexythiazox, 2% for Etoxazole, 10% for Coumaphos, 3% for Pridaben, 5% for Propargite, 8% for Spirodiclofen, 1% for Fenpyroximate.2.An analytical method for the determination of 10 acaricides by LC-MS/MS in royal jelly 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. The linear ranges were from 0.1-200μg/L for 10 acaricides and the correlation coefficients(r2)were all greater than 0.99. The blank royal jelly sample spiked in four concentrations at 5、10、50、100 μg/kg, the recoveries ranged from 73%-107%, and the ralative standard deviations ranged from 0.9% to 12.5%. The decision limits ranged from 0.25 to 1.0μg/kg, and the detection capabilities ranged from 0.75 to 3.9μg/kg. The Propargite was detected in one royal jelly samples among 10 samples.