Determination of spinosad at trace levels in bee pollen and beeswax with solid-liquid extraction and LC-ESI-MS

作者:Yanez Karen P; Martin Maria T; Bernal Jose L; Nozal Maria J; Bernal Jose
来源:Journal of Separation Science, 2014, 37(3): 204-210.
DOI:10.1002/jssc.201301069

摘要

This paper reports the use of a new LC method with a fused-core analytical column coupled to ESI-MS to determine residues of the biopesticide spinosad in bee pollen and beeswax. The method analyzes the active ingredients, spinosyns A and D, with a simple and efficient sample treatment (recovery between 90 and 105%) consisting of a solid-liquid extraction with acetone (bee pollen) or acetonitrile (beeswax). The method was validated in terms of selectivity, LOD, LOQ, linearity, and precision. The LOD and LOQ values ranged between 0.1-0.2 and 0.4-0.7 mu g/kg, respectively. Moreover, the precision obtained within the linear concentration range (LOQ 500 mu g/kg) was satisfactory (RSD lower than 5%). Finally, the proposed method was applied to analyze bee pollen and beeswax samples collected from apiaries located close to fruit orchards in two Spanish regions.

  • 出版日期2014-2