摘要
【目的】建立气相色谱快速检测植物性食品中氟啶虫酰胺残留量的方法。【方法】对气相色谱检测方法中植物性食品提取溶剂、凝胶渗透色谱净化技术（GPC）收集时间、固相萃取小柱、气相色谱柱等进行了分析,建立了检测植物性食品中氟啶虫酰胺残留量的方法,并对该方法的检测范围、检测低限进行分析,最后用建立的方法测定了7种植物性食品的添加回收率及精密度。【结果】建立的检测植物性食品中氟啶虫酰胺残留量的方法为：将样品用乙酸乙酯均质提取,提取液经凝胶渗透色谱仪（净化收集时间为7~14 min）和氨基SPE小柱净化,乙酸乙酯定容,用带DB-1701毛细管柱气相色谱仪进行分析。氟啶虫酰胺质量浓度为10~500μg/L时,其质量浓度与峰面积呈现良好的线性关系,相关系数为0.999,由此计算得出氟啶虫酰胺的检测低限为10μg/kg。氟啶虫酰胺添加量为10,20,100,400μg/kg时,7种植物性食品的添加回收率在82.0%~116.0%,标准偏差为0.06~3.17,精密度较高。【结论】建立的氟啶虫酰胺残留量检测方法快速、简便、经济,准确性和灵敏度都非常高。
【Objective】 The study was to establish a rapid method to determine flonicamid residues in seven kinds of plant-based foods by gas chromatography.【Method】 In this method,experiments on the extraction solvents,gathering time by GPC,solid phase extraction cartridges and columns of GC were carried out.And,a rapid method to determine flonicamid residues in plant-based foods by gas chromatography was established.The detection range and the limit of low detection of the method were also studied,while the recoveries and the precision of flonicamid were analyzed too.【Result】 The established method to determine flonicamid residues in plant-based foods by gas chromatography demonstrated that the samples were homogenized and extracted with ethyl acetate,and extracts were loaded into GPC（gathering time 7-14 min）.Eluent was cleaned up with NH2 SPE cartridge.The final purified extract of food was analyzed by GC with DB-1701.The result showed that the limit of low detection was 10 μg/L.There was a good linear relationship between the peak area value and the concentration of flonicamid within range of 10-500 μg/L（correlation coefficient=0.999）.When the spiked concentration of flonicamid was 10,20,100,400 μg/kg respectively,the recoveries ranged from 82.0%-116.0%.The standard deviations ranged from 0.06-3.17 with a high precision.【Conclusion】 This method is simple,inexpensive,accurate and sensitive.
出处
《西北农林科技大学学报（自然科学版）》
CSCD
北大核心
2011年第3期82-86,91,共6页
Journal of Northwest A&F University(Natural Science Edition)
基金
广州市科技攻关重大项目(2006Z1-E0121)
