摘要
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。
Objective 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 （150 mm×4.6 mm, 5 μm） column with methanol-water （pH4.5） （85 ： 15）, （87 ： 13） as mobile phase with a flow rate of 1.0 ml/min, respectively. The benzo （a） pyrene and 3-hydroxybcnzo （a） pyrene were detected under FD at λex/λem = 265 nm/450 nm, λex/λem = 365 nm/450 nm with an injection volume of 20 μ1, respectively. Results Benzo （a） pyrene was linear in range of 0. 1- 10. 0 ng/ml, r =0. 999 4 and 3-hydroxybenzo （a） pyrene was linear in range of 1.07 100. 7 ng/ml, r = O. 992 1. For benzo （a） pyrene and 3-hydroxybenzo （a） pyrene, the limit of quantification was O. 1μg/ kg, 0.2 μg/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.
出处
《中国食品卫生杂志》
北大核心
2013年第2期152-154,共3页
Chinese Journal of Food Hygiene
基金
国家自然科学基金资助项目(30770724)
