Journal
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
Volume 33, Issue 3, Pages 442-451Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2015.1128565
Keywords
HPLC-MS/MS; hull; kernel; neonicotinoid; sunflower seed; thiamethoxam; translocation
Funding
- Spanish Ministry Economia y Competitividad
- INIA [RTA2013-00042-C10-03, 06]
- University of Valladolid [CIP13/04]
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A validated analytical method to determine seven neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid and thiacloprid) in sunflower seeds (hull and kernel) using HPLC coupled to electrospray ionisation mass spectrometry (ESI-MS) is presented. Sample clean-up based on a solid-liquid extraction, and the removal of lipid fraction, in the case of kernels, is proposed and optimised. Low limits of detection and quantification were obtained, ranging from 0.3x10(-3) to 1.2x10(-3)mu gg(-1) and from 1.0x10(-3) to 4.0x10(-3)mu gg(-1), with good precision, and recovery values ranged from 90% to 104% for hulls and kernels. The method was applied for the analysis of five thiamethoxam-dressed sunflower seeds and four non-treated seeds, where, besides thiamethoxam, residues of the other neonicotinoid, clothianidin, were also detected and confirmed via tandem mass spectrometry (LC-ESI-MS/MS). Finally, the presence of residues of thiamethoxam and clothianidin in collected sunflower seeds (hulls) coming from coated seeds confirmed the translocation of these neonicotinoids through the plant up to these seeds.
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