高效液相色谱法测定食用植物油中苯并(a)芘的研究

Determination of benzo(a)pyrene in edible vegetable oil by high performance liquid chromatography

目的建立食用植物油中苯并(a)芘的固相萃取-高效液相色谱荧光检测器测定方法。方法样品以正己烷溶解,用3种不同苯并(a)芘专用固相萃取柱进行样品净化,经Waters PAH C18色谱柱分离后,用高效液相色谱荧光检测器测定,峰面积外标法定量食用植物油中苯并(a)芘含量。结果苯并(a)芘浓度在0~38.5 ng/m L范围内,浓度与色谱峰面积呈良好的线性关系,线性相关系数为0.9998,检出限为0.1μg/kg。在添加量为5.5~11.0.0μg/kg时,经3种Ba P专用SPE小柱处理的回收率均在91.7%~109.2%之间,测定结果的相对标准偏差为2.84%~3.26%(n=6)。结论以上几种处理方法均适用于食用植物油中苯并(a)芘的日常检测,但总体讲小柱3的实用性更强,并有更好的应用前景。

ABSTRACT:Objective A high performance liquid chromatography (HPLC) was developed for the determination of benzo(a)pyrene (BaP) in edible oil.Methods The sample was dissolved and extracted by hexane, and then purified by 3 different kinds of cleanert BaP solid phase extraction (SPE) cartridge, respectively. The HPLC separation was performed on a Waters PAH C18 column with acetonitrile and water as mobile phase. The BaP was determined by fluorescence detection, and quantified by the peak area external standard method. Results A good linearity was obtained in the range of 0~38.5 ng/mL for BaP with the correlation coefficient was 0.9998. The limit of detection (LOD) was 0.1μg/kg for BaP in edible oil. When spiked with 5.5~11.0.0μg/kg, the recoveries of BaP purified by 3 different kinds of cleanert BaP-SPE cartridge sranged from 91.7% to 109.2%%. The relative standard deviation (RSD) was 2.84%~3.26% (n=6). Conclusion The above treatment methods can be used for the routine analysis of BaP in edible oil. But on the whole, the practicability of the cleanert BaP-SPE cartridges③ was better, which has a good application prospect.