Determination of Insecticide of Phenylpyrazole Derivatives in Poultry Derived Foods by QuEChERS Method Combined with Liquid Chromatography-Mass Spectrometry
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摘要: 本方法建立了一种QuEChERS-液质联用法同时检测禽源性食品中氟虫腈、氟甲腈、氟虫腈砜、氟虫腈亚砜、乙虫腈、丁烯氟虫腈共6种苯基吡唑类杀虫剂残留的方法。样品采用乙腈提取、QuEChERS方法净化,质谱采集模式为ESI-negative--MRM。结果表明,6种苯基咪唑类杀虫剂在不同基质中的定量限不同,定量限范围为0.06~1.20 μg/kg,在不同线性范围(1~40、4~160、10~400 μg/kg)下相关性良好(R2>0.994)。考虑三类样品基质的区别,分别进行3种水平的标准添加测试,回收率达84.49%~107.86%,相对标准偏差为0.99%~4.19%。该方法快速、灵敏、准确,适合用于禽源性食品中苯基咪唑类杀虫剂残留量的测定。
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关键词:
- 苯基吡唑类 /
- 禽源性食品 /
- QuEChERS /
- 液相色谱-质谱联用法
Abstract: A method for determination of the content of six kinds of insecticide of phenyrazole derivatives including fipronil,fipronil-desulfinyl,fipronil-sulfone,fipronil-sulfide,ethiprole,flufiprole in poultry derived foods by QuEChERS method combined with liquid chromatography-mass spectrometry detection was established. The samples were extracted with acetonitrile,and purified with QuEChERS. The mass spectrometry analysis used ESI-negative-MRM method. The results showed that,the LOQs of six find of phenylpyrazole derivatives were different in samples of different matrixes,the LOQs range were 0.06~1.20 μg/kg.It was showed good linearities(R2>0.994)in different ranges of 1~40,4~160,10~400 μg/kg.Considering the difference of three kinds of sample,three levels of addition tests were carried out,the average recoveries were 84.49%~107.86%,the relative standard deviation(RSD)were 0.99%~4.19%. The method was rapid,sensitive and precise,and could be suitable for determination of insecticide of phenylpyrazole derivatives in poultry derived food. -
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