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Determination of spinosad at trace levels in bee pollen and beeswax with solid–liquid extraction and LC – ESI ‐ MS
Author(s) -
Yáñez Karen P.,
Martín María T.,
Bernal José L.,
Nozal María J.,
Bernal José
Publication year - 2014
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201301069
Subject(s) - beeswax , chromatography , extraction (chemistry) , bee pollen , chemistry , acetone , apiary , solid phase extraction , high performance liquid chromatography , pollen , beekeeping , wax , botany , biology , organic chemistry
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 μg/kg, respectively. Moreover, the precision obtained within the linear concentration range (LOQ 500 μg/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.