固相萃取/高效液相色谱荧光法测定水产品中苯并芘

采用Florisil固相萃取柱纯化样品,建立了高效液相色谱(HPLC)荧光法测定水产品中苯并(a)芘的方法.样品以正己烷为提取剂,净化、蒸发浓缩后用流动相溶解.荧光检测器激发波长297 nm,发射波长405 nm.流动相为V(乙腈):V(水)=75:25,流速1.0 mL/min,外标法定量.苯并(a)芘在0～200 ng/mL浓度范围内线性关系良好,相关系数r=0.99990;在5个空白样品中添加0.5μg/kg浓度水平的标准品,回收率在81.9%～89.5%之间,相对标准偏差为4.1%(n=5);日内、日间精密度分别为0.7%(n=5)、2.4%(n=3);最低检测限为90 ng/kg.

The study on determination of benzopyrene in aquatic products by SPE/high performance liquid chromatography with fluorescence detection

A method was developed for the determination of benzopyrene in aquatic products by high performance liq-uid chromatography with fluorescence detection. The method involved solid phase extraction of benzopyrene from aquat-ic products. After being extracted with n-hexane, purified using a Florisil SPE column and concentrated by evapora-tion, the residue was dissolved in the mobile phase which consisted of acetonitrile (75%) and water (25%), and then detected at λ_(ex), 297 nm, λ_(em) 405 nm with the flow rate at 1.0 mL/min. Finally, the benzopyrene was quantified by external standard method. When spiked with 0.5 μg/kg benzopyrene in 5 blank samples, the recoveries were 81.9%～89.5% with the RSD of 4.1% (n = 5). The method showed good linearity over the range of 0～200 ng/mL for benzopyrene with correlation coefficient of 0.99990, the detection limit of 90 ng/kg, the intm-and inter-day preci-sion of 0.7 % (n = 5) and 2.4 % (n = 3). The method is applicable for the detection of benzopyrene in aquatic prod-ucts. The sensitivity, accuracy and precision have all met the analysis requirement.