液相色谱法测定油性食品中苯并(α)芘的方法改进

Improvement of determining benzo(α) pyrene in greasy food by high performance liquid chromatography

采用Florisil固相萃取柱净化样品,建立了高效液相色谱(HPLC)荧光法测定食品中苯并(α)芘的方法。样品以环己烷为提取剂,净化、蒸发浓缩后用流动相溶解。荧光检测器激发波长283 nm,发射波长404 nm。流动相为V(乙腈)∶V(水)=85∶15,流速1.0 mL/min,外标法定量。苯并(α)芘在0～100 ng/mL浓度范围内线性关系良好,相关系数r2=0.9998;方法的测定低限:橄榄油、罗非鱼和猪肉均为1.0μg/kg,添加浓度1.0～100μg/kg,其回收率范围81.0%～93.2%,变异系数0.65%～6.15%。

The samples were extracted by florisil solid phase,and the benzo（α） pyrene in food was determined by High Performance Liquid chromatography combined with fluorescence method.The samples were saponified with cyclohexane as an extraction solvent,and purified,evaporated and concentrated.Then,the samples were dissolved in mobile phase,and detected by fluorescence detector,with excitation wavelength 283 nm,emission wavelength 404 nm.The volume fraction of the mobile phase was 15（water）：85（acetonitrile）.Its flow speed was 1.0 mL/min.The concentration of Benzo（α） pyrene in the range of 0 ~100 ng / mL showed a good linear relationship,its correlation coefficient r2=0.9998.The determination of lower limit was,olive oil,tilapia and pork were used 1.0 μg/kg and added 1.0 ~100 μg/kg.The recovery rate was 81.0% ~93.2%,and the coefficient of variation was 0.65% ~6.15%.