分散固相萃取净化/高效液相色谱法测定婴幼儿奶粉与米粉中15种多环芳烃

Determination of Polycyclic Aromatic Hydrocarbons in Infant Formula and Rice by High Performance Liquid Chromatography with Dispersive Solid Phase Extraction Purification

建立了高效液相色谱-荧光检测法同时测定婴幼儿奶粉和米粉中15种多环芳烃的检测方法。样品经乙腈提取,PSA分散固相萃取净化;乙腈-水梯度洗脱,Waters PAH专用柱分离,荧光检测器检测,外标法定量。在最优条件下,15种多环芳烃均得到有效分离,线性范围为1.0~50μg/L,相关系数均大于0.995,方法检出限(LODs,S/N=3)为0.05~0.3μg/kg,回收率为86.5%~106.8%,精密度(RSD,n=6)为0.7%~7.5%。该方法操作简单、灵敏度高,适用于婴幼儿奶粉和米粉中多环芳烃的检测。

An analytical method was established for the determination of 15 polycyclic aromatic hydrocarbons （PAHs ） in infant formula and rice by high performance liquid chromatography with fluorescence detector （HPLC-FLD ）.The samples were extracted with acetonitrile,purified by PSA dispersed solid phase extraction,separated on a Waters PAH special column with acetonitrile-water as mobile phase by gradient elution,and detected with the fluorescence detector.These compounds were quantified by the external standard method.Under the optimal conditions,15 PAHs were effectively separated.The linear ranges were 1.0-50 μg/L with correlation coefficients above 0.995.The limits of detection （ S/N =3 ） for 15 PAHs were between 0.05 μg/kg and 0.3 μg/kg.The recoveries were in the range of 86.5 % -106.8 % with relative standard deviations （ n =6 ） of 0.7 % -7.5 % .The method was simple and highly sensitive,and was suitable for the determination of polycyclic aromatic hydrocarbons in infant formula and rice.