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目的为了结合《蜂蜜卫生标准》的修订要求中补充农药残留等相关指标和检验方法的需要,建立气相色谱法同时测定蜂蜜中10种拟除虫菊酯类农药残留的方法。方法通过对毛细管柱的类型、溶剂的种类、固相萃取小柱种类的选择实验,确定应用二氯甲烷为提取溶剂,经弗罗里硅土固相萃取柱净化,DB-17(0.25 mm×0.25μm×20 m)的毛细管柱作为分离柱,以GC-ECD测定,峰面积定量。结果 10种农药加标回收率为77.3%~103.0%,相对标准偏差2.5%~7.5%,检出限为0.000 5~0.005 mg/kg(当称样量为5.00 g时)。结论该方法适合蜂蜜中多种拟除虫菊酯类农药残留的同时检测。
OBJECTIVE To establish a method for the simultaneous determination of 10 pyrethroid pesticide residues in honey by gas chromatography in order to meet the need of supplementing indicators and test methods of pesticide residues in the revised requirements of Honey Health Standard. Methods Based on the selection of capillary column type, solvent type and solid phase extraction cartridge type, dichloromethane (dichloromethane) was selected as the extraction solvent and purified by Florisil SPE. DB-17 (0.25 mm × 0.25 μm × 20 μm) was used as the separation column to determine the peak area by GC-ECD. Results The spiked recoveries of 10 pesticides ranged from 77.3% to 103.0% with relative standard deviations from 2.5% to 7.5% with a detection limit of 0.0005 to 0.005 mg / kg (when the sample weight was 5.00 g). Conclusion This method is suitable for the simultaneous detection of many pyrethroid pesticide residues in honey.