分子印迹固相萃取–高效液相色谱法的优化及在测定植物油中苯并(a)芘含量的应用

Optimization of Molecularly Imprinted Solid Phase Extraction-High Performance Liquid Chromatography and Its Application in Determination of Benzo(a)pyrene in Vegetable Oil

建立优化的分子印迹固相萃取超高效液相色谱法测定植物油中苯并芘的检测方法。实验过程中通过对样品不同固相萃取净化效能、最佳检测波长、流动相体系及色谱柱使用的考察,结果表明,分子印迹固相萃取净化柱比较适合植物油样品的前处理萃取及净化,最佳检测波长为激发波长365 nm和发射波长410 nm,苯并芘色谱峰在此条件下具有较高的响应值和信噪比,在90%乙腈–10%水流动相体系下,目标峰具有较好的分离效果,采用150 mm的短柱子能有效提高工作效率。苯并芘在浓度0.3~20μg/L范围内具有良好的线性关系,相关系数大于0.9999,方法检出限为0.05μg/kg,定量限为0.10μg/kg,3个添加浓度水平的平均回收率为87.6%~95.9%,相对标准偏差为1.08%~2.16%。实际样品检测中,苯并芘的检出率为39.0%,超标率为2.4%,合格率为97.6%。该优化方法灵敏度高,操作便捷,快速准确,可适用于植物油中苯并芘的批量检测及污染监测情况分析。

An optimized method for the determination of benzopyrene in vegetable oil by molecular imprinting solid phase extraction with ultra-high performance liquid chromatography was established.During the experiment,through the investigation of different solid-phase extraction purification efficiency,optimal detection wavelength,mobile phase system and chromatographic column use,the results showed that the molecularly imprinted solid phase extraction purification column was more suitable for pretreatment extraction and purification of vegetable oil.The optimal detection the excitation wavelength and the emission wavelength were 365 nm and 410 nm,respectively.Under these conditions,the benzopyrene chromatographic peak had high response value and signal-to-noise ratio.Under the mobile phase system of 90%acetonitrile-10%water,the target peak had a good separation effect.Using 150 mm short columns can effectively improve work efficiency.Benzopyrene had a good linear relationship in the concentration range of 0.3~20μg/L,and the correlation coefficient was greater than 0.9999.The detection limit and quantitative limit of benzopyrene determination method were 0.1μg/kg and 0.3μg/kg,respectively.The average recoveries of three added concentrations were 87.6%~95.9%,and the relative standard deviations were 1.08%~2.16%.In the actual sample detection,the detection rate of benzopyrene,the exceeding rate and the qualified rate were 39.0%,2.4%,and was 97.6%,respectively.This optimization method is sensitive,convenient,rapid and accurate,and can be used for batch detection of benzopyrene in vegetable oil and analysis of pollution monitoring.