凝胶色谱净化-超高效液相色谱法测定食用油中苯并芘残留

Determination of Benzo(a) Pyrene Residue in Cooking Oil by Gel Permeation Chromatography Cleanup and Ultra Performance Liquid Chromatography

建立了凝胶色谱净化-超高效液相色谱(GPC-UPLC)测定食用油中苯并芘的分析方法。样品用V_(乙酸乙酯):V(环己烷)=1:1提取,去除大分子油脂。以BEH C18柱(1.7μm,2.1 mm×50 mm)为分离柱,V_(乙腈):V_水=88:12为流动相,在优化试验条件下,苯并芘的检出限为0.05μg/kg,定量限为0.1μg/kg,苯并芘的线性范围为0.1～10μg/kg,相关系数为0.997。样品在0.1,0.2及10μg/kg三个加标水平的加标回收率为70.1%～97.5%,相对标准偏差为0.9%～10.7%。该方法灵敏度高、自动化程度高,可用于食用油中苯并芘的常规检测。

A new method for the accurate assay of benzo（a）pyrene in cooking oil by permeation chromatography cleanup and ultra high performance liquid chromatography （GPC-UPLC） with fluorence detection is established. Cooking oil samples are extracted by Vethyl acetate： Vcyclohexane=1 ： 1, and then purified by gel permeation chromatography to eliminate the macromolecular grease. The UPLC analysis is performed on a BEH C18 column （1.7 μm, 2.1 mm × 50 mm） with a mobile phase of Vacetoritile ： VH2O =88 ： 12. Under the optimal conditions, the calibration curve is linear in the range of 0.1-10 μg/kg, with correlation coefficient of 0.997. The limit of detection （LOD） is 0.05 μg/kg. The recovery results at three concentration levels （0.1, 0.2, 10μg/kg） are all in the range of 70.1%-97.5% with RSDs ranging from 0.9%-10.7%. The proposed method is sensitive and highly automatic. It is suitable for the routine determination of benzo（a）pyrene in cooking oil.