基于SPE-HPLC的芹菜中环境雌激素检测

目的]建立芹菜茎叶中6种环境雌激素（雌酮、17β-雌二醇、雌三醇1、7α-乙炔基雌二醇、双酚A和4-壬基酚）的高效液相色谱检测方法。方法]样品切碎榨汁后,用超声波振荡提取,固相萃取小柱浓缩净化,对硝基苯甲酰氯柱前衍生,高效液相色谱法荧光测定。结果]6种环境雌激素的线性范围为8.3～1 000.0μg/L,相关系数r=0.998 8～0.999 9,最低检出限量为3.7～8.3μg/L。样品加标平均回收率在89.60%～97.13%,相对标准偏差RSD均小于2.9%。结论]该研究建立的方法同时测定芹菜茎叶中的6种环境雌激素,结果满意。

Determination of Environmental Estrogens from Celery Stem and Leaf by Solid Phase Extraction and High Performance Liquid Chromatography

Objective] To establish a high performance liquid chromatographic method(HPLC) for the simultaneous determination of environmental estrogens including estriol,17β-estradiol,estrone,17α-ethinyl estradiol,bisphenol A and 4-nonylphenol in celery stem and leaf.Method] After the sample smashed and pressed out the juice,the target compounds were concentrated using ultrasonic extraction,and purified with the solid phase extraction column,and detected by the highly performance liquid chromatography after solid phase extraction and pre-colum fluoresent dirivatization with p-nitrobenzoyl chloride.Result] The linear range of the method is from 8.3 to 1 000.0 μg/L(r=0.999 8-0.999 9).The detection limits of the method were from 3.7 to 8.3 μg/L.The recoveries were from 89.60% to 97.13%.All of the relative standard deviations were under 2.9%.Conclusion] The method has been applied to the detection of the 6 kinds of environment estrogen from celery samples with satisfactory results.