| Avermectin,ivermectin and albendazole are commonly used antiparasitic drugs in the process of livestock and poultry breeding.Irregular use will cause excessive veterinary drug residues in animal products,which will cause a series of harm to consumers.At present,high performance liquid chromatography-photo-diode array（HPLC-PDA）method for simultaneous detection of abamectin,ivermectin,albendazole and its three metabolite residues in beef,chicken and eggs has not been reported yet.In this study,QuEChERS and liquid-liquid extraction（LLE）methods were used to extract the target compounds.Development and optimization of HPLC-PDA method for simultaneous detection of abamectin（AVM）,ivermectin（IVM）,albendazole（ABZ）,albendazole sulfone（ABZ-SO2）,albendazole sulfoxide（ABZ-SO）and albendazole-2-aminosulfone（ABZ-2NH2-SO2）residues in beef,chicken,and eggs（whole eggs,egg whites and egg yolks）.The main findings of this study are shown as follows:1.A method for simultaneous extraction of the AVM,IVM,ABZ,ABZ-SO2,ABZ-SO and ABZ-2NH2-SO2 residues in beef and chicken muscle by using QuEChERS technology.That is,10 mL acetonitrile was added to the sample,vortex and oscillation.Subsequently,QuEChERS reagent（4 g anhydrous magnesium sulfate,1 g sodium chloride,1.5 g sodium citrate buffer）was added to the sample.Vortex quickly and centrifuge,the supernatant was collectted.The sample solution was centrifugal concentration and then re-dissolved with the initial mobile phase.The recoveries of the six target compounds were all greater than 85.10%by using this method.2.A method for simultaneous extraction of the AVM,IVM,ABZ,ABZ-SO2,ABZ-SO and ABZ-2NH2-SO2 residues in egg by using LLE method.That is,extractant solution（acetonitrile:water,90:10,v/v）was added to the sample for vortex and vibration,the precipitate was then removed by centrifugation,repeated extraction once.The combined supernatants were concentrated by centrifugal concentrator and then re-dissolved with the initial mobile phase.The recoveries of the six target compounds were all over 85.70%by using this method.3.A HPLC-PDA method for simultaneous detection of AVM,IVM,ABZ,ABZ-SO2,ABZ-SO and ABZ-2NH2-SO2 residues in beef,chicken muscle and egg was established and optimized.XBridgeTM C18 column（4.6 mm×150 mm,5 μm）was used,0.1%trifluoroacetic acid-aqueous and methanol were used as the mobile phase.The target compounds were separated by gradient elution at a flow rate of 1.0 mL/min,the column temperature was 30℃.The detection wavelengths of ABZ and three metabolites of ABZ were 302.0 nm and 288.0 nm,respectively;the detection wavelengths of AVM and IVM were all 244.0 nm.The results of this study showed that the concentration range of ABZ,ABZ-SO2,ABZ-SO,ABZ-2NH2SO2 and AVM were at the limit of quantitation（LOQ）～600.0 μg/L,the concentration range of IVM were at the LOQ～400.0μg/L,the peak area of the targets have a good linear relationship with its concentration,and the determination coefficient（R2）were both greater than 0.999 0.When added the concentrations of ABZ,ABZ-SO2,ABZ-SO,ABZ-2NH2-SO2,AVM and IVM were LOQ,0.5 MRL,1.0 MRL and 2.0 MRL,the recoveries in blank beef and chicken muscle were 88.78%-93.43%,85.10%～93.27%,91.67%～96.64%,86.06%～94.42%,91.08%～95.04%and 90.62%～96.10%,respectively;the intra-day relative standard deviation（RSD）were 1.47%～3.47%,1.44%～4.03%,1.52%～4.30%,2.47%～4.53%,1.99%～4.51%and 1.83%～3.23%,respectively;the inter-day RSD were 1.81%～3.83%,1.89%～4.86%,1.68%～4.65%,2.65%～4.93%,1.95%～4.78%and 1.35%～4.37%,respectively;the limits of detection（LODs）were 9.8～12.5 μg/kg,8.3～9.0μg/kg,3.6～4.2μg/kg,3.3～4.0μg/kg,8.7～8.8μg/kg and 3.2～4.5 μg/kg,respectively;and the LOQs were 28.6～30.0μg/kg,24.1～26.5 μg/kg,10.2～12.0μg/kg,9.5～11.4μg/kg,25.5～25.8μg/kg and 9.0～11.2μg/kg,respectively;the recoveries in blank egg were 88.91%～95.37%,87.76%～96.39%,89.96%～96.23%,90.13%～97.21%,85.70%～93.29%and 87.79%～94.47%,respectively;the intra-day RSD were 1.49%～3.16%,1.29%～3.69%,1.62%～3.98%,1.76%～4.15%,2.14%～4.08%and 1.44%～3.25%,respectively;the inter-day RSD were 1.32%～4.07%,1.74%～4.85%,1.66%～4.60%,2.06%～4.33%,2.71%～4.82%and 1.70%～3.76%,respectively;the LODs were 8.6～10.5 μg/kg.6.0～7.8μg/kg,2.1～3.2μg/kg,2.8～3.6 μg/kg,7.9～8.6μg/kg and 2.8～3.5μg/kg,respectively;and the LOQs were 25.0～28.4 μg/kg,20.0～22.1μg/kg,7.8～8.1μg/kg,10.6～12.4μg/kg,25.0～26.4μg/kg and 9.5～11.4 μg/kg,respectively.This method is fast and efficient,and provides a new detection method for the simultaneous detection of ABZ,ABZ-SO2,ABZSO,ABZ-2NH2-SO2,AVM and IVM residues in animal-derived foods. |
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