高效液相色谱-荧光检测法测定螺旋藻中苯并[a]芘残留

Determination of Benzo[a]pyrene in Spirulinaby High Performance Liquid Chromatography-Fluorescence Detection

建立了高效液相色谱-荧光检测法测定螺旋藻中苯并[a]芘残留的分析方法。螺旋藻样品用正己烷提取,经中性Al2O3固相萃取（SPE）柱净化。用Zorbax Eclipse XDB-C18色谱柱分离,流动相为乙腈-水（85∶15,V/V）,流速1.0mL/min,荧光检测器检测。苯并[a]芘的质量浓度在0~20ng/mL范围内线性关系良好,相关系数r=0.9999,检出限为0.12μg/kg,定量限为0.40μg/kg,回收率为96.60%~101.2%,相对标准偏差为1.38%~5.68%。该方法准确,灵敏度高,重复性好,适用于螺旋藻中苯并[a]芘残留的测定。

A method was established based on solid phase extraction-high performance liquid chromatography（HPLC）with fluorescence detection to determine the residues of benzo[a]pyrene in the Spirulina.The benzo[a]pyrene in the Spirulina was extracted by n-hexame,and purified with neutral Alumina column as filler.The mobile phase was consisted of acetonitrile and water（85∶15,V/V）with the flow rate at 1.0mL/min.Good linearity was achieved in the range of 0-20ng/mL for benzo[a]pyrene with correlation coefficient of 0.9999,the limit of detection was 0.12μg/kg and the limit of quantification was 0.40μg/kg.The mean recoveries of benzo[a]pyrene were in the range of 96.60%-101.2% with relative standard deviations from 1.38%to 5.68%.The method is accurate,sensitive,repeatable and can be used for the analysis of benzo[a]pyrene in Spirulina.