Zhongguo youzhi (Apr 2023)
全自动固相萃取净化-高效液相色谱法测定 食用植物油中苯并（a）芘含量Determination of benzo(a)pyrene in edible vegetable oil by automated solid phase extraction-high performance liquid chromatography
Abstract
为提高工作效率，降低误差，建立分子印迹柱全自动固相萃取净化-高效液相色谱法测定食用植物油中苯并（a）芘含量的方法。样品经正己烷提取，采用全自动固相萃取仪进行分子印迹柱净化，C18色谱柱分离，高效液相色谱-荧光检测器检测。结果表明：苯并（a）芘在0.5~20.0 ng/mL质量浓度范围内与峰面积线性关系良好，相关系数为 0.999 9，方法检出限为0.09 μg/kg，定量限为0.30 μg/kg，加标回收率为91.7%~111.8%，相对标准偏差为2.0%~8.2%，与国标方法的检测结果不存在显著性差异；对市售38份食用植物油样品进行检测发现，苯并（a）芘的检出率为76.3%。该方法准确度高、重复性好，可批量自动化前处理样品，提高工作效率，并降低人员操作误差风险，适用于食用植物油中苯并（a）芘含量的测定。 In order to improve work efficiency and reduce errors, a molecularly imprinted column automated solid phase extraction-high performance liquid chromatography method for determination of benzo(a)pyrene content in edible vegetable oil was established. The benzo(a)pyrene in samples was extracted using n-hexane, purified by automated solid phase extraction instrument with molecularly imprinted column, separated by C18 column and detected by high performance liquid chromatography with a fluorescence detector. The results showed that benzo (a) pyrene had a good linear relationship with peak area in the range of 0.5-20.0 ng/mL, with a correlation coefficient of 0.999 9. The limit of detection was 0.09 μg/kg, and the limit of quantitation was 0.30 μg/kg. The average recovery rate was 91.7%-111.8% with the relative standard deviation of 2.0%-8.2%. In the detection of edible vegetable oil, there was no significant difference between the established method and the national standard method.Afterwards, the method was applied to determine the benzo(a)pyrene content in commercial 38 edible vegetable oil samples, and the detection rate was 76.3%. In conclusion, the method is highly accurate and repeatable, and can improve the efficiency using batch automation preprocessing, reduce the risk of personnel operation error, and is suitable for the measurement of benzo(a) pyrene content in edible vegetable oil.
Keywords
