分子印迹固相萃取-同位素稀释气相色谱质谱法测定肉制品中16种欧盟优控多环芳烃

Determination of 16 European priority polycyclic aromatic hydrocarbons in meat products by the molecularly imprinted solid phase extraction-isotope dilution-gas chromatography mass spectrometry

结合分子印迹固相萃取对多环芳烃的特异性净化,建立了同位素稀释气相色谱质谱法测定肉制品中16种欧盟优控多环芳烃的分析方法.样品加入7种氘代同位素内标,经正己烷+二氯甲烷(7:3,V/V)混合溶液提取,分子印迹固相萃取柱净化,选择离子监测模式(SIM)下采集.在1.0—200 ng·mL^(−1)范围内,16种欧盟优控多环芳烃线性相关系数(r)均大于0.9990,不同加标浓度下,回收率为87.1%—114.8%,相对标准偏差(RSDs)(n=6)在1.0%—5.5%范围内,方法的检出限为0.2—0.3μg·kg^(−1),定量限为0.6—0.9μg·kg^(−1).方法前处理简单高效,灵敏度高,适用大批量肉制品中多环芳烃的快速测定.

Based on the specific purification of the molecularly imprinted solid phase extraction,a method for the determination of 16 EU priority polycyclic aromatic hydrocarbons(PAHs)in meat products by isotope dilution-gas chromatography mass spectrometry was established.Seven deuterium isotope internal standards were added to the samples,which were extracted by a mixture of n-hexane-dichloromethane(7:3,V/V).The samples were purified by the molecular imprinting column,separated by the DB-EUPAH column,collected in select ion monitoring mode(SIM),and quantified by the internal standard method.In the range of 1.0—200 ng·mL^(−1),the linear correlation coefficients (r^(2)) were all greater than 0.9990, the average recoveries were in the range of 87.1%- 114.8% and the relative standard deviations (RSDs) (n=6) were ranged from 1.0% to 5.5%. The detection limits of the method were 0.2-0.3 μg·kg^(−1) and the limits of quantification were 0.6- 0.9 μg·kg^(−1) respectively. The method is simple, efficient, sensitive and suitable for the rapid determination of the EU PAHs in meat products.