高级检索

    高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量

    Rapid Determination of Residual Amount of Benzo(a)pyrene in Fruit-Vegetable Chips by High Performance Liquid Chromatography

    • 摘要: 建立了高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量的方法。样品经正己烷提取,苯并(a)芘分子印迹柱净化后,经Eclipse Plus C18色谱柱(150 mm×4.6 mm,5.0 μm)分离,以体积分数为90%的乙腈溶液为流动相进行等度洗脱。结果表明:苯并(a)芘的质量浓度与其对应的峰面积在0.4~100 μg·L-1内呈线性关系,相关系数为0.999 9。测定下限(10S/N)为0.40 μg·kg-1。以果蔬脆片样品为基质在3个浓度水平下进行加标回收试验,所得日内回收率为89.4%~93.7%,测定值的相对标准偏差(n=6)为4.3%~7.2%;日间回收率为87.6%~92.5%,测定值的相对标准偏差(n=6)为5.8%~8.4%。用此方法分析了20个果蔬脆片样品,在7个样品中检出了苯并(a)芘,但其含量均小于GB 2762-2017规定的限量(10 μg·kg-1)。

       

      Abstract: A method for the rapid determination of residual amount of benzo(a)pyrene residues in fruit-vegetable chips with high performance liquid chromatography was developed. The fruit-vegetable chip sample was extracted with n-hexane, and then purified with benzo(a)pyrene molecularly imprinted column. The sample solution obtained was separated with a Eclipse Plus C18 chromatographic column (150 mm×4.6 mm, 5.0 μm), and eluted isocratically with using acetonitrile solution with volume fraction of 90% as mobile phase. Results were found that the linearity relationship between mass concentration of benzo(a)pyrene and its respective peak area was kept in the range of 0.4-100 μg·L-1, with correlation coefficient of 0.999 9. Lower limit of determination (10S/N) found was 0.40 μg·kg-1. The spiked recovery was made at 3 concentration levels by using fruit-vegetable chip samples as matrix, giving recoveries (n=6) of inter-day and intra-day in the ranges of 89.4%-93.7% and 87.6%-92.5%, with RSDs (n=6) of determined values of inter-day and intra-day in the ranges of 4.3%-7.2% and 5.8%-8.4%, respectively. The prescribed method was used in analyzing the 20 fruit-vegetable chip samples, and benzo(a)pyrene was found in 7 samples, with content all lower than limit (10 μg·kg-1) specified by GB 2762-2017.

       

    /

    返回文章
    返回