双柱在线净化系统快速检测动植物油脂中的苯并(a)芘

Determination of benzo (a) pyrene in animal and vegetable oils by double columns on-line purification

该文建立了双色谱柱在线净化-超高速液相色谱仪联用检测动植物油脂(猪油、花生油、茶籽油、大豆油、调和油)中苯并(a)芘方法。采用正己烷-异丙醇溶液提取试样中苯并(a)芘,提取液过滤后进样,利用试验组建的双色谱柱系统进行在线净化,第一根色谱柱为分离、富集柱,采用Kromasil反C18(4.6 mm×150 mm,5μm)柱;第二根色谱柱负责进一步分离苯并(a)芘,采用Chrom Spher pi(80 mm×3.0 mm,5μm)色谱柱。试验结果表明,样品中苯并(a)芘含量在1.0~20.0 ng/mL,与峰面积呈良好线性关系,相关系数r2为0.9996,检出限为0.08μg/kg,在1.00、5.00、10.00μg/kg加标水平下,加标回收率为82.0%~91.6%,相对标准偏差为1.89%~4.29%。该方法可用于常见动植物油脂等易受苯并(a)芘污染的样品的快速检测。

A method for the determination of benzo(a)pyrene in animal and vegetable oils(lard,peanut oil,camellia seed oil,soybean oil and blending oil)by on-line purification with dualcolumn and ultra-high-speed liquid chromatography was established.Benzo(a)pyrene was extracted by n-hexane-isopropanol solution,filtered and injected into the sample,and purified on-line by the dual-column system.The first column was used as separation and enrichment column,Kromasil anti-C18(4.6 mm×150 mm,5μm)column was used;the second column was responsible for further separation and separation of benzo(a)Pyrene was separated by Chrom Spher PI(80 mm×3.0 mm,5μm)column.The results showed that the content of benzo(a)pyrene in the sample had a good linear relationship with the peak area in the range of 1.0-20.0 ng/mL.The correlation coefficient R2 was0.9996,and the detection limit was 0.08μg/kg.Under the standard addition levels of 1.00,5.00 and 10.00 g/kg,the recovery rate was 82.0%-91.6%,and the relative standard deviation was 1.89%-4.29%.This method could be used for the rapid detection of samples contaminated by benzo(a)pyrene such as animal and vegetable oils.