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食品研究与开发:2022,43(20):179-185
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气相色谱法测定食用植物油中有机氯类农药残留
(1.天津食品集团有限公司,天津 300000;2.君乐宝乳业集团农业农村部乳品质量安全控制重点实验室,河北 石家庄 050021;3.天津康复疗养中心,天津 300191)
Determination of Organochlorine Pesticide Residues in Edible Vegetable Oil by Gas Chromatography
(1.Tianjin Food Group Co.,Ltd.,Tianjin 300000,China;2.Key Laboratory of Dairy Quality and Safety Control,Ministry of Agriculture and Rural Affairs,Junlebao Dairy Group,Shijiazhuang 050021,Hebei,China;3.Tianjin Rehabilitation Convalescent Center,Tianjin 300191,China)
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投稿时间:2022-04-11    
中文摘要: 以大豆油为代表性基质,建立气相色谱测定食用植物油中18种有机氯农药残留的方法。测定方法为样品经过提取液(乙腈)超声提取,离心取上清液,上清液经C18填料净化,40℃旋转蒸干,加入1.00 mL正己烷复溶,用毛细管柱气相色谱分离,电子捕获检测器检测,以保留时间定性,峰高或峰面积定量。18种有机氯农药在5 ng/mL~60 ng/mL线性相关性良好,相关系数均大于 0.995,定量限为 5 μg/kg~16 μg/kg,在添加量为 5 μg/kg~20 μg/kg 的加标回收试验下,18种有机氯农药的加标回收率范围为80.3%~118.3%。精密度验证所得相对标准偏差为1.8%~12.7%。因此,该方法满足实验室要求,可用于定性及定量检测食用植物油中18种有机氯农药残留。
Abstract:This study aims to develop a gas chromatography method for the determination of 18 organochlorine pesticide residues in edible vegetable oil.Specifically,soybean oil was tested and the sample was extracted by sonication with acetonitrile and centrifuged.The supernatant was collected and purified with C18 packing,followed by rotary evaporation to dryness at 40℃and reconstitution with 1.00 mL n-hexane.The yielded product was separated by capillary column gas chromatography and detected by electron capture detector.The pesticide residues were qualified by retention time and quantified by peak height or peak area.The 18 organochlorine pesticides showed good linearity in the range of 5 ng/mL-60 ng/mL and the correlation coefficients were all>0.995.The limits of quantification fell in the range of 5 μg/kg-16 μg/kg.At the spiked levels of 5 μg/kg-20 μg/kg,the recovery of the 18 organochlorine pesticides ranged from 80.3% to 118.3%.The precision test showed that the relative standard deviation of the obtained results was 1.8%-12.7%.Therefore,this method has high accuracy,which can be used for qualitative and quantitative detection of 18 organochlorine pesticide residues in edible vegetable oil.
文章编号:202220023     中图分类号:    文献标志码:
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