Research and Development Department of Nederland Co, Viladecans, Barcelona, Spain.
Pest Manag Sci. 2010 Nov;66(11):1230-5. doi: 10.1002/ps.1999.
The purpose of this work was to determine residues of acaricides in recycled Spanish beeswax.
Chlorfenvinphos, fluvalinate, amitraz, bromopropylate, acrinathrin, flumethrin, coumaphos, chlorpyrifos, chlordimeform, endosulfan and malathion residues were determined by GC-µECD/NPD/MS detection. Owing to the extreme instability of amitraz, this analyte was transformed into the stable end-metabolite 2,4-dimethylaniline, later derivatised with heptafluorobutyric anhydride and determined by GC-µECD/MS. Recoveries from spiked samples ranged from 86 to 108%, while quantification limits varied from 0.10 to 0.30 mg kg(-1) using GC-µECD/NPD, and from 12 to 85 µg kg(-1) by GC-MSD. Of a total of 197 samples analysed, only eight samples (4%) were free of residues of chlorfenvinphos (0.019-10.6 mg kg(-1)), fluvalinate was present in 93.6% of samples analysed (0.027 -88.7 mg kg(-1)), while coumaphos was confirmed in only five of the 134 samples analysed at concentrations of less than 195 µg kg(-1). The remaining acaricides were identified with different levels of incidence at concentrations from 12 to 231 µg kg(-1).
Residues of acaricides were found in an extensive number of beeswax samples. The contamination with chlorfenvinphos and tau-fluvalinate was very relevant, particularly as chlorfenvinphos is not legally authorised for use in beekeeping. The possible impacts of the main acaricides detected on larval and adult honey bees are discussed.
本研究旨在检测回收西班牙蜂蜡中的杀螨剂残留。
采用 GC-µECD/NPD/MS 检测,确定了氯芬威、氟螨嗪、甲胺磷、溴丙脒、丙体六六六、氟氯氰菊酯、扑灭司林、毒死蜱、双甲脒、硫丹和马拉硫磷残留。由于甲胺磷极度不稳定,将其转化为稳定的末端代谢物 2,4-二甲基苯胺,然后用全氟丁基酐衍生化,采用 GC-µECD/MS 进行测定。加标样品的回收率为 86%108%,GC-µECD/NPD 的定量限为 0.100.30mgkg(-1),GC-MSD 为 1285µgkg(-1)。在所分析的 197 个样品中,只有 8 个样品(4%)不含氯芬威(0.01910.6mgkg(-1))残留,93.6%的样品中含有氟螨嗪(0.02788.7mgkg(-1)),在分析的 134 个样品中,只有 5 个样品中含有 195µgkg(-1)以下的灭蝇胺残留。其余杀螨剂以不同的浓度水平存在,浓度为 12231µgkg(-1)。
在大量蜂蜡样品中发现了杀螨剂残留。氯芬威和噻螨酮的污染非常严重,特别是氯芬威在养蜂中未被合法授权使用。讨论了检测到的主要杀螨剂对幼虫和成年蜜蜂的潜在影响。