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

Abstract

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.

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

“…In addition, there is a large number of articles demonstrating validation of LC-ESI-MS methods for practical analytical tasks with respect to certain validation guidelines such as FDA [68][69][70][71][72], ICH [73][74][75] Eurachem [76][77][78][79][80][81][82][83], EMA [84][85][86], IUPAC [87][88][89] or SANCO [90,91]. However, in most cases not all parameters are investigated.…”

Analysis of Intact Glucosinolates in Beeswax by Liquid Chromatography Tandem Mass Spectrometry

“…Nevertheless, the preferable and simplest choice is a solvent extraction with heated water or mixtures of methanol and water (Ares et al 2014;Bell et al 2015;Domínguez-Perles et al 2010;Glauser et al 2012;López-Berenguer et al 2008;Millán et al 2009;Rochfort et al 2008). Consequently, taking into account our experience and the favorable results obtained in recent research (Ares et al 2015;Yáñez et al 2014), we decided to use solvent extraction as the sample treatment. Analysis of intact GLSs was usually performed by LC with ultraviolet or diode array (Ares et al 2014;Gratacós-Cubarsí et al 2010;López-Berenguer et al 2008;Rochfort et al 2006;Truchado et al 2010;) and mass spectrometry (MS) (Alarcón-Flores et al 2013;Ares et al 2014;Bell et al 2015;Domínguez-Perles et al 2010;Glauser et al 2012;López-Berenguer et al 2008;Millán et al 2009;Rochfort et al 2008;Sasaki et al 2012) detectors, while C 18 analytical columns were used in most cases.…”

“…In view of the absence of specific procedures in which intact GLSs were determined in beeswax, it was decided that a solvent extraction should be developed and optimized as the sample treatment; this decision was the result of the simplicity of this extraction procedure and our experience with it (Ares et al 2015;Yáñez et al 2014). Firstly, consideration was given to the amount of beeswax to be analyzed.…”

Development and validation of a liquid chromatography with mass spectrometry method to determine resveratrol and piceid isomers in beeswax

“…However, several other sample treatments have been employed to analyze stilbenes, such as solvent extraction , MAE or ultrasound‐assisted extraction , SFE , or PLE . Furthermore, the current trend in sample preparation techniques is focused on the simplification of those procedures to reduce the number or reagents and time spent on this step . Thus, the use of microextraction or stir bar sorptive extraction has become popular in recent years to determine stilbenes.…”

“…Thus, the use of microextraction or stir bar sorptive extraction has become popular in recent years to determine stilbenes. Some of those sample treatments could be used in beeswax, but taking into account our experience and the good results obtained in recent research , we decided to use solvent extraction as the sample treatment.…”