固相萃取-高效液相色谱法分析食用油中的苯并芘

Determination of the Benzo(a)pyrene level in cooking oil by solid phase extraction-high performance liquid chromatography

目的建立一种高效液相色谱-荧光检测器检测食用油中苯并芘的方法。方法对济南市场上食用油中苯并芘含量进行调查分析,采用SHIMADZU shim-pack VP-ODS(250 mm×4.6 mm,5μm)色谱柱,以甲醇∶水(90∶10,V/V)为流动相,流速为1.0 mL/min,样品使用无键合硅胶固相萃取柱处理后,在激发波长285 nm、发射波长406 nm处进行检测。结果方法的最低检出限(S/N=3)为0.039μg/kg,样品的加标回收率为85.8%～90.7%,日内精密度为2.9%～4.1%,日间精密度为3.7%～5.3%。结论该方法灵敏度高,选择性好,定量准确,适用于食用油中苯并芘的检测。

Objective To establish a high performance liquid chromatography with fluorescence detector for the determination of the benzo（a）pyrene（B（a）P） level in the cooking oil.Methods The difference of B（a）P content in edible oil in Jinan market was investigated by the SHIMADZU shim-pack VP-ODS（250 mm×4.6 mm,5 μm） column.The mobile phase was methanol-water（90∶ 10,V/V）,and the flow rate was 1.0 mL/min.The samples were treated by the non-bonded silica solid phase extraction（SPE） column,and then detected at the 285 nm excitation wavelength and 406nm emission wavelength.Results The lowest limit of determination was 0.039 μg/kg（S/N=3）.The recovery rate was 85.8%-90.7%,and the intra-day and inter-day relative standard deviations were 2.9%-4.1% and 3.7%-5.3%.Conclusion This method is high sensitive,good selective and quantitative accurate,which is suitable for the B（a）P determination in the cooking oil.