知识与财富的链接
目的 建立检测海产品中苯并(a)芘(BaP)及其代谢产物3-羟基苯并芘(3-OHBaP)的高效液相色谱荧光法(HPLC-FD).方法 样品经65％乙腈提取,涡旋混匀,离心沉淀,分别以甲醇-水(pH 4.5)(85∶ 15)、(87∶ 13)为流动相进行色谱分离BaP、3-OHBaP,色谱柱为Century SIL C18-BDS(150 mm×4.6 mm,5μm),流速1.0 ml/min;荧光检测器检测BaP激发波长265 nm,发射波长450 nm,检测3-OHBaP激发波长365 nm,发射波长450 nm;进样量20μl.结果 BaP在0.1～10.0 ng/ml浓度范围内线性关系良好,相关系数r=0.999 4;3-OHBaP在1.07 ～100.7 ng/ml浓度范围内线性关系良好,相关系数r=0.992 1.BaP、3-OHBaP回收率分别在96.8％～ 112.0％、72.6％～ 83.3％之间;相对标准偏差分别为6.0％、5.2％(n=5);最低检测限分别为0.1和0.2μg/kg.结论 该法简便、快速、灵敏度高,可用于海产品中BaP及其代谢产物3-OHBaP的检测.
An analytical method for the determination of benzo(a)pyrene and its metabolite 3-hydroxybenzo(a)pyrene in seafood was developed by high performance liquid chromatography with fluorescence detection (HPLC-FD).Methods The samples were extracted by 65% acetonitrile, treated by vortex blending and centrifugal precipitation. For benzo(a)pyrene and 3-hydroxybenzo(a)pyrene, the chromatographic separation were achieved in CenturySIL C18-BDS(150mm×4.6mm, 5μm)column with methanol-water(pH 4.5)(85∶15),(87∶13)as mobile phase with a flow rate of 1.0ml/min, respectively. The benzo(a)pyrene and 3-hydroxybenzo(a)pyrene were detected under FD at λex/λem=265nm/450nm, λex/λem=365nm /450nm with an injection volume of 20μl, respectively.Results Benzo(a)pyrene was linear in range of 0.1～10.0ng/ml,r=0.9994and 3-hydroxybenzo(a)pyrene was linear in range of 1.07～100.7ng/ml,r=0.9921. For benzo(a)pyrene and 3-hydroxybenzo(a)pyrene, the limit of quantification was 0.1μg/kg, 0.2μg/kg, the recoveries were 96.8%～112.0%, 72.6%～83.3%, and the relative standard deviations was 6.0%, 5.2%(n=5), respectively.Conclusion The method is simple,rapid and highly sensitive. It is suitable for the determination of benzo(a)pyrene and 3-hydroxybenzo(a)pyrene in seafood.
