固相萃取/高效液相色谱荧光法测定水产品中苯并芘

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

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。

A method was developed for the determination of benzopyrene in aquatic products by high performance liquid chromatography with fluorescence detection. The method involved solid phase extraction of benzopyrene from aquatic products. After being extracted with n-hexane, purified using a Florisil SPE column and concentrated by evaporation, the residue was dissolved in the mobile phase which consisted of acetonitrile （75 % ） and water （25 % ）, and then detected at λex 297 nm, λem 405 nm with the flow rate at 1.0 mL/min. Finally, the benzopyrene was quantified by external standard method. When spiked with 0.5μg/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 intra- 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.