Gbylik-Sikorska Malgorzata, Sniegocki Tomasz, Posyniak Andrzej
Pharmacology and Toxicology Department, National Veterinary Research Institute (NVRI), al. Partyzantow 57, 24-100 Pulawy, Poland.
Pharmacology and Toxicology Department, National Veterinary Research Institute (NVRI), al. Partyzantow 57, 24-100 Pulawy, Poland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 May 15;990:132-40. doi: 10.1016/j.jchromb.2015.03.016. Epub 2015 Apr 1.
The original analytical method for the simultaneous determination and confirmation of neonicotinoids insecticides (imidacloprid, clothianidin, acetamiprid, thiametoxam, thiacloprid, nitenpyram, dinotefuran) and some of their metabolites (imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, desnitro-imidacloprid hydrochloride, thiacloprid-amid and acetamiprid-N-desmethyl) in honey bee and honey was developed. Preparation of honey bee samples involves the extraction with mixture of acetonitrile and ethyl acetate followed by cleaned up using the Sep-Pak Alumina N Plus Long cartridges. Honey samples were dissolved in 1% mixture of acetonitrile and ethyl acetate with addition of TEA, then extracts were cleaned up with Strata X-CW cartridges. The identity of analytes was confirmed using liquid chromatography tandem mass spectrometry. All compounds were separated on a Luna C18 column with gradient elution. The whole procedure was validated according to the requirements of SANCO 12571/2013. The average recoveries of the analytes ranged from 85.3% to 112.0%, repeatabilities were in the range of 2.8-11.2%, within-laboratory reproducibility was in the range of 3.3-14.6%, the limits of quantitation were in the range of 0.1-0.5μgkg(-1), depending of analyte and matrices. The validated method was successfully applied for the determination of clothianidin, imidacloprid and imidacloprid urea in real incurred honey bee samples and clothianidin in honey.
建立了同时测定和确证蜜蜂及蜂蜜中新烟碱类杀虫剂（吡虫啉、噻虫胺、啶虫脒、噻虫嗪、噻虫啉、烯啶虫胺、呋虫胺）及其某些代谢物（吡虫啉胍、吡虫啉烯烃、吡虫啉脲、脱硝基吡虫啉盐酸盐、噻虫啉酰胺和啶虫脒 -N-去甲基物）的原始分析方法。蜜蜂样品的制备包括用乙腈和乙酸乙酯的混合物进行萃取，然后使用Sep-Pak Alumina N Plus Long柱进行净化。蜂蜜样品用含三乙胺的1%乙腈和乙酸乙酯混合物溶解，然后提取物用Strata X-CW柱进行净化。使用液相色谱串联质谱法确证分析物的身份。所有化合物在Luna C18柱上进行梯度洗脱分离。整个程序根据SANCO 12571/2013的要求进行了验证。分析物的平均回收率在85.3%至112.0%之间，重复性在2.8 - 11.2%范围内，实验室内再现性在3.3 - 14.6%范围内，定量限在0.1 - 0.5μgkg(-1)范围内，具体取决于分析物和基质。该验证方法成功应用于实际受污染的蜜蜂样品中噻虫胺、吡虫啉和吡虫啉脲的测定以及蜂蜜中噻虫胺的测定。
