混合离子液体-静态顶空气相色谱法测定转基因大豆油中六六六与滴滴涕残留量

Simultaneous Determination of HCH and DDT Residues in Transgenic Soybean Oil by Mixed Ionic Liquids-Static Headspace Gas Chromatography

基于离子液体无蒸气压、高沸点、溶解能力优良及混合离子液体同时具有亲水和疏水性的特点,建立了以[Bmim]PF6∶[Bmim]BF4为1∶2的混合离子液体作为顶空溶剂,平衡加压静态顶空进样测定转基因大豆油中六六六、滴滴涕残留量的方法.对离子液体的种类、配比、用量,以及顶空平衡温度、顶空平衡时间、顶空进样时间等条件进行了优化.研究结果表明：在最佳条件下,方法的线性范围为5～100μg/L,相关系数为0.9905～0.9996,检出限为1.4～15.2 μg/kg,定量下限为4.7～48.6 μg/kg,回收率为72.3％～104.1％,相对标准偏差为0.6％～7.8％.本方法快速、准确,且避免了复杂的前处理,是顶空进样检测农残的新方法.

A balance pressure static headspace sampling gas chromatographic method was developed for the determination of HCH and DDT pesticide residues in the transgenic soybean oil using a typical mixed ionic liquids of [Bmim] PF6-[Bmim] BF4 by a ratio of 1 ∶ 2 as a headspace solvent,based on that mixed ionic liquids have the characteristics of low vapor pressure,high boiling point,excellent dissolving ability,good hydrophilicity and hydrophobicity at the same time.Experimantal conditions,including type of ionic liquid,proportion and dosage of ionic liquid,headspace equilibration temperature,headspace equilibration time and headspace sampling time were optimized.The results showed that the calibration curves were linear in the range of 5-100 μg/L,with correlation coefficients of 0.990 5-0.999 6.The detection limits and quantitation limits of 8 pesticides were in the range of 1.4-15.2 μg/kg and 4.7-48.6 μg/kg,respectively.The recoveries and RSDs were 72.3％-104.1％ and 0.6％-7.8％,respectively.The method was rapid and accurate,and could be uesed to avoide for the complicated sample pretreatment process.