二维液相色谱法测定烧烤肉制品中苯并(a)芘

烧烤肉制品由于富含动物油脂,在炭火高温烧烤熟制品过程中,容易出现苯并(a)芘超标问题,具有较高安全隐患。建立二维液相色谱仪检测烧烤肉制品中苯并(a)芘的方法。第1维为分离、富集柱,采用InertsilODS柱(4.6mm×150mm,5μm),流动相为乙腈-水(85∶15,V/V),流速1.0mL/min,可以实现500μL样品中目标物苯并(a)芘的富集与分离;第2维采用ChromSpherPi柱(3.0mm×80mm,5μm),流动相为异丙醇-乙腈(60∶40,V/V),流速1.2mL/min,可以有效分离、测定样品中的苯并(a)芘。结果表明:烧烤肉制品中苯并(a)芘在1.0~20.0ng/mL范围内呈线性关系,其线性回归方程为y=1.8471x-0.1033(r=0.999),检出限为0.08μg/kg,在1.00、3.00、5.00、10.00μg/kg加标水平下,加标回收率为97.1%~105.2%,相对标准偏差为1.55%~2.77%。

Determination of Benzo(a)pyrene in Barbecued Meat Products by Two-Dimensional Liquid Chromatography

During the high-temperature grilling of barbecued meat products over charcoal fire, the problem of benzo(a)pyrene production in amounts exceeding the safety limit occurs easily due to their richness in animal fat, which is a high potential safety hazard. A method for the determination of benzo(a)pyrene in barbecued meat products by two-dimensional liquid chromatography was established. The first dimension allowed the separation and enrichment of benzo(a)pyrene from 500 μL of samples using an Inertsil ODS (4.6 mm ×150 mm, 5 μm) column with a mobile phase consisting of acetonitrilewater (85:15, V/V) at a 1.0 mL/min flow rate;the second dimension was intended to effectively separate and detect benzo(a)pyrene in samples using a ChromSppi column (3.0 mm × 80 mm, 5 μm) with a mobile phase consisting of isopropanol-acetonitrile (6:4, V/V) at a flow rate of 1.2 mL/min. The results showed that the linear regression equation was y=1.847 1x-0.103 3 (correlation coefficient r = 0.999) with good linearity over the concentration range of 1.0–20.0 ng/mL. The detection limit was 0.08 μg/kg. The recovery of benzo(a)pyrene spiked at concentration levels of 1.00, 3.00, 5.00 and 10.00 μg/kg was 97.1%–105.2% with relative standard deviation (RSD) of 1.55%–2.77%.