Multi-residue method for the confirmation of four avermectin residues in food products of animal origin by ultra-performance liquid chromatography–tandem mass spectrometry

Abstract

A confirmatory method was developed for the rapid determination of abamectin, ivermectin, doramectin and eprinomectin residues in various food products of animal origin, such as pork muscle, pork liver, fish and milk. Samples were homogenized, extracted and de-proteinized by acetonitrile, cleaned via two-step cleaning procedure using Bond Elut C₁₈ SPE columns and then alumina-N cartridges. All the four avermectin residues in different animal-food products were simultaneously separated and determined by ultra-performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC–ESI–MS/MS) within 3.5 min. Data acquisition under positive ESI–MS/MS was performed by applying multiple reaction monitoring (MRM) for both identification and quantification, and mass spectrometric conditions were optimized to increase selectivity and sensitivity. The matrix-matched calibration curves for different matrices, such as pork muscle, pork liver, fish and milk, were constructed and the interference effect of different sample matrices on the ionization was effectively eliminated. The UPLC–MS/MS method was validated with satisfactory linearity, recovery, precision and stability. Matrix-matched calibration curves of abamectin, ivermectin, doramectin and eprinomectin in four different matrices were linear (r²≥ 0.990, goodness-of-fit coefficients ≤12.8%) in the range 2.5–200 µg kg⁻¹. The limits of detection and quantification for the four avermectins were in the range 0.05–0.68 and 0.17–2.27 µg kg⁻¹, respectively. Recoveries were 62.4–104.5% with good intra- and inter-day precision. The method was rapid, sensitive and reliable, and can be applied to the quantitative analysis of avermectin residues in different animal-food products.

Keywords:

• chromatography, HPLC, LC/MS
• drug residues, ivermectin
• animal products, meat
• milk

Acknowledgements

Financial support from the National Natural Scientific Foundation of China (20905017), the Key Project of Commonweal Programs for Marine Science (201005034-3), the Primary Scientific Foundation of FIO (2010G25), the Scientific Foundation of Shandong Entry-Exit Inspection and Quarantine Bureau (SK200621) and the Science Foundation for Youth Scholars of State Oceanic Administration (2010140) is gratefully acknowledged.