固相萃取-高效液相法测定芝麻油中苯并(a)芘

Determination of Benzo(a) Pyrene in Sesame Oil by Solid-phase Extraction Coupled with High Performance Liquid Chromatography

建立一种快速、高效测定芝麻油中苯并(a)芘的固相萃取-高效液相色谱(SPE-HPLC)方法。样品前处理采用硅胶固相萃取柱串联氧化铝固相萃取小柱,稀释液和淋洗液选择正己烷,洗脱液选择二氯甲烷,在40℃下氮吹干后,乙腈复溶后检测。采用Waters RP C18色谱柱(4.6 mm×250 mm,5μm)分离,以乙腈-水(90∶10)作为流动相,用荧光检测器检测,外标法峰面积定量。结果表明,苯并(a)芘在1.00 ng/m L^20.00 ng/m L浓度范围内线性良好,相关系数r2为0.999 8,检出限为0.05μg/kg,定量限为0.16μg/kg,加标回收率达到92.2%~98.5%。

A rapid and effective method was established for the determination of benzo(a)pyrene in sesame oil by solid-phase extraction coupled with high performance liquid chromatography(SPE-HPLC). The samples were treated by silica gel SPE tandem alumina solid-phase extraction column,and the leaching solution of n-hexane,the eluent of dichloromethane. The elution liquid was dried at 40 ℃ under nitrogen,and detected after re-dissolution with acetonitrile.The separation of targeted compound was performed on a Waters RP C18 chromatographic column(4.6 mm×250 mm,5 μm)using acetonitrile-water(90 ∶ 10)as mobile phase,with fluorescence detector and external standard method peak area quantification. The linear range of benzo(a)pyrene was in the range of 1.00 ng/m L-20.00 ng/m L with a correlation coefficient of 0.999 8.The detection limit was 0.05μg/kg and the quantitative limit was 0.16 μg/kg. The recovery rate was 92.2 %-98.5 %.