串联分子印迹固相萃取-高效液相色谱法测定食用油中苯并(a)芘

Determination of benzo(a)pyrene in cooking oil by tandem molecularly imprinted solid phase extraction-high performance liquid chromatography

目的建立一种分子印迹固相萃取-高效液相色谱法测定食用油中苯并(a)芘的含量的分析方法。方法在GB 5009.27-2016《食品中苯并(a)芘的测定》试样处理方法基础上,进一步使用Welchrom~?Silica硅胶固相萃取小柱串联Welchrom~?BAP-2分子印迹固相萃取小柱对多种食用油基质进行净化。试样中目标物采用Ultimate~?XB-C_(18)(4.6 mm×250 mm, 5μm)色谱柱分离,以乙腈和水(88:12, V:V)为流动相进行等度洗脱,于激发波长370nm、发射波长425nm处进行检测。结果食用油试样经串联固相萃取小柱净化,除杂的效果好、回收率高。线性范围为1.0～100.0μg/mL,线性相关系数r在为0.9999,回收率在88.7%～101.3%之间,检出限为0.5μg/kg。结论本文建立的方法简便、灵敏度高、准确性好,适用于食品中苯并(a)芘的定性定量分析。

Objective To establish a method for determination of benzo(a)pyrene in edible oil by molecularly imprinted solid phase extraction-high performance liquid chromatography.Methods Based on the sample processing method of GB 5009.27-2016 Determination of benzo(a)pyrene in foods,Welchrom?Silica silica solid phase extraction cartridges were connected in series with Welchrom?BAP-2 molecularly imprinted solid phase extraction cartridges for purification several edible oil.The target in the sample was separated by a Ultimate?XB-C18(4.6 mm×250 mm,5μm)column.The acetonitrile and water(88:12,V:V)was used as mobile for isocratic elution,and the sample was detected at an excitation wavelength of 370 nm and an emission wavelength of 425 nm.Results The results showed that cascaded SPE column provided good impurity elimination and high recovery on cooking oil sample.The calibration curves showed a good linearity with correlation at 0.9999.The linear range for the quantification of benzo(a)pyrene were 1.0-100.0μg/mL.The recoveries of the method were 88.7%-101.3%.The limits of detection were 0.5μg/kg.Conclusion This method is simple,sensitive,accurate and is suitable for the quantitative analysis of the benzo(a)pyrene in edible oil samples.