气相色谱法测定蜂蜜中10种拟除虫菊酯类农药残留
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卫生部《蜂蜜安全标准》起草项目组课题


Determination of pyrethroid pesticide residues in honey by gas chromatography
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    摘要:

    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。

    Abstract:

    Objective In order to fulfill the requirement of revising and adding more determination methods and indexes for pesticide residues in the Hygienic Standard for Honey,and to establish a method of detecting 10 pyrethroid pesticide residues simultaneously in honey by GC.Methods Through comparing the type of capillary columns,solvents and solid phase extract columns,it was decided to have the extraction with dichloromethane,cleaned-up with Florisl solid phase extract column,and separation with capillary column DB-17(0.25 mm×0.25 μm×20 m).The residues were quantified with GC-ECD and the area of peaks.Results The recoveries of fluvalinate residues were 77.3%-103.0%,the RSDs were 2.5%-7.5%,the detection limits were 0.000 5-0.005 mg/kg(as the quantity of sample was 5.00 g).Conclusion The method was easy to handle and separate each component,and suitable for the simultaneous analysis of 10 pyrethorid pesticide residues in honey.

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林国斌,倪蕾,林升清.气相色谱法测定蜂蜜中10种拟除虫菊酯类农药残留[J].中国食品卫生杂志,2012,24(2):116-119.

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