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,5 μm)柱;第二根色谱柱负责进一步分离苯并(a)芘,采用 ChromSpher pi(80 mm×3.0 mm,5 μm) 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0.999 6,检出限为 0.08 μg/kg,在1.00、5.00、10.00 μg/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 dual-column 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, 5 μm) 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, 5 μm) 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 was 0.999 6, and the detection limit was 0.08 μg/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.
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