Study On Simultaneous Determination Of Pesticide And Veterinary Drug Residues In Bee Products

In recent years, people have had a keen awareness of health and natural health products. Withthe increasing of consumption levels, people in world, demand more bee products. The qualityand safety of bee products have been taken seriously. This paper studied the simultaneousdetermination of pesticide and veterinary drug residues in beehives and honey matrixs.This topic research includes two parts:(1) Selective Multi-Residue Analysis Method. A simple and effective method wasdeveloped for the simultaneous determination of chlortetracycline (CTC), oxytetracycline (OTC),tetracycline (TC) and doxycycline (DC) in beehives using liquid chromatography-triplequadrupole mass spectrometry (LC-MS/MS). Analytes were extracted in EDTA-McIlvainebuffer from beehives by ultrasonication and shaking, purified using hexane distribution and HLBcartridges, quantified using a matrix-matched standard calibration curve, and validated accordingto Commission Decision2002/657/EC and SANCO/10684/2009. The responses were linear inthe range of1to500μg L-1amount to concentration of0.2to100μg kg-1based on5g of samplewith correlation coefficients (r2)>0.99. The overall recoveries were in the range of73.8to106.7%with RSD of1.19to9.8%. The limits of quantification (LOQ) were1μg kg-1for CTCand DC and0.2μg kg-1for OTC and TC. The decision limits (CCα) ranged from0.041to0.31μg kg-1, and the detection capabilities (CCβ) ranged from0.064to0.43μg kg-1. The applicationof this method revealed low concentrations of OTC and TC in some real beehive samples.(2) Multi-class, Multi-Residue Analysis Method. To simultaneously determinatesulfadiazine, sulfathiazole, sulfadimidine (sulfonamide), norfloxacin, ciprofloxacin,(quinolones)oxytetracycline, tetracycline (tetracyclines), chloramphenicol (Amphenicol), coumaphos(acaricide) in honey, an LC-MS/MS method was developed and validated. The extraction andpurification were based on SPE and MSPD. Accuracy and precision were validated at1,1.5,2MRL levels (coumaphos at0.5,1,1.5MRL levels) and the overall recovery was between88.29and110.91%, and RSD <10%. The LOD was in the rage of0.05to2μg kg-1and the LOQ in therange of0.75to10μg kg-1.