气相色谱质谱联用法测定饲料原料中16种多环芳烃

Determination of 16 Polycyclic Aromatic Hydrocarbons in Feed Materials by Gas Chromatography-Mass Spectrometry

本研究建立了一种气相色谱质谱联用法定量测定饲料原料中16种多环芳烃的方法。以D10-苊、D12-■和D12-苯并(a)芘为内标物,对饲料原料中的多环芳烃提取、净化和定量方法进行优化。结果表明,在2~1 000 ng/mL范围内,16种多环芳烃峰面积与内标物峰面积比值均与质量浓度比值呈良好线性关系,相关系数均大于0.999;检出限和定量限分别为0.6~1.2、1.8~3.6μg/kg;在2、5、20μg/kg三个加标水平下,回收率在75.6%~94.8%之间,相对标准偏差在0.8%~11.9%之间。该方法净化效果好、灵敏度高、重复性好,具有较强的复杂基质抗干扰能力,可用于批量饲料原料样品中的多环芳烃的定量测定。

A gas chromatography-mass spectrometry method for qualitative and quantitative determination of 16 polycyclic aromatic hydrocarbons in feed materials was developed.D 10-Acenaphthene,D 12-Chrysene and D 12-benzo(a)pyrene were selected as the internal standard substances to optimize the extraction method,purification method and quantitative method of 16 polycyclic aromatic hydrocarbons in feed materials.The results indicated that the ratio of the peak area of 16 polycyclic aromatic hydrocarbons to the peak area of internal standard showed a good linear relationship with the mass concentration in the range of 2~1000 ng/mL,and the coefficients of association were larger than 0.999.The detection limits and quantitation limits of 16 polycyclic aromatic hydrocarbons were 0.6~1.2μg/kg and 1.8~3.6μg/kg respectively.The average recoveries at the addition levels of 2.0、5.0μg/kg and 20.0μg/kg were 75.6%~94.8%.The relative standard deviations are 0.8%~11.9%(n=6).The sensitive,effective and reproducible method can be used for quantitative determination of 16 polycyclic aromatic hydrocarbons in batch feed material samples.