Isolation and multiresidue detection of macrolide endectocides present in animal matrices.

Abstract

A simple, rapid, and sensitive method for isolation and detection of macrolide endectocides (moxidectin, doramectin, selamectin, ivermectin, and eprinomectin) in animal sera and liver is described. Fortified sera or homogenized liver samples were treated with sodium chloride followed by organic solvent extraction. No additional steps were required prior to analysis. Separation of analytes and collection of mass information was achieved by liquid chromatography/mass spectrometry with positive atmospheric pressure chemical ionization set in selected ion monitoring mode with each sample analysis complete in 15 minutes. Presence of each compound was confirmed based on 2 separate extracted ion profiles. Detection of avermectins and moxidectin in a range of working standards was achieved at 10, 50, and 100 ppb. Quantitation of these compounds in fortified samples was based on standard calibration curves with R2 > 0.99. Detection limits of 10 ppb for ivermectin, moxidectin, and doramectin, 50 ppb for selamectin, and 100 ppb for eprinomectin were achieved in spiked sera. Recoveries of avermectins and moxidectin in 500 ppb fortified sera fell between 61 and 89% (+/-5.7-15.7). Analysis of fortified liver gave comparable results with recovery of selamectin of 83-91% +/- 18.3. A complete mass spectral fragmentation pattern of selamectin and affordable screening method for 6 macrolide endectocides are reported. Method comparison for salt treatment and solid-phase extraction of fortified samples is discussed.