Competence Center for Residue Analysis, Austrian Agency for Health and Food Safety, Spargelfeldstrasse 191, 1220 Wien, Austria.
J Agric Food Chem. 2011 Dec 14;59(23):12271-7. doi: 10.1021/jf202775m. Epub 2011 Nov 11.
An analytical method for the simultaneous determination of residues of eight neonicotinoid insecticides and two metabolites in honey using LC-MS/MS was developed and validated. Two approaches of sample preparation were investigated, with the final method involving acetonitrile extraction and subsequent cleanup by dispersive solid-phase extraction (QuEChERS type). Validation was based on quintuplicate analysis at three fortification levels and showed satisfactory recoveries (60-114%) and high precision (RSDs between 2.7 and 12.8%). Low limits of detection and quantification could be achieved for all analytes ranging from 0.6 to 5 μg/kg and from 2 to 10 μg/kg, respectively. Investigations of Austrian honey samples revealed the presence of acetamiprid, thiacloprid, and thiamethoxam residues in honey; however, no sample exceeded the maximum residue limits. On average, flower honey samples contained neonicotinoid residues in higher quantities compared to forest honey samples.
建立并验证了一种利用 LC-MS/MS 同时测定蜂蜜中 8 种新烟碱类杀虫剂和 2 种代谢物残留的分析方法。研究了两种样品前处理方法，最终方法采用乙腈提取，随后用分散固相萃取（QuEChERS 型）进行净化。验证基于 3 个加标水平的 5 次重复分析，结果表明回收率良好（60%-114%），精密度高（RSD 为 2.7%-12.8%）。所有分析物的检测限和定量限均较低，范围分别为 0.6-5μg/kg 和 2-10μg/kg。对奥地利蜂蜜样品的调查发现，蜂蜜中存在乙酰甲胺磷、噻虫啉和噻虫嗪残留；但没有样品超过最大残留限量。平均而言，与森林蜂蜜样品相比，花蜂蜜样品中含有更多的新烟碱类杀虫剂残留。
