中空纤维膜液相微萃取-液相色谱法测定己烯雌酚
目的 建立鸡肉中己烯雌酚残留的中空纤维膜液相微萃取-液相色谱分析方法。方法 对影响萃取富集效率的实验条件进行优化, 采用聚丙烯中空纤维膜, 以叔丁基甲基醚为萃取溶剂, 萃取溶剂用量20 μL, 萃取温度35 ℃, 萃取时间30 min, 搅拌速率为500 r/min, 萃取液40 ℃水浴, 氮气吹干后用流动相溶解, 取10 μL进行液相色谱检测。结果 该方法对己烯雌酚的富集倍数为40倍, 己烯雌酚在7.814~97.670 μg/mL质量浓度范围内线性关系良好, 相关系数均大于0.99, 检测限(S/N=3)为2.0 μg/kg, 实际样品中的加标回收率为78.07%~ 88.46%, 相对标准偏差为0.99%~8.36%。结论 本方法灵敏、简便, 适用于鸡肉中己烯雌酚残留的检测。
Objective To establish an analytical method for the determination of diethylstilbestrol in chicken by hollow fiber-based liquid phase microextraction coupled with high pressure liquid chromatography(HPLC). Methods Some main experimental parameters that affected the extraction efficiency were optimized. Methyl tert-butyl ether 20 μL was selected as both the extraction solvent and the impregnation solvent. The extraction was carried out at 35 ℃ with a stirring rate of 500 r/min for 30 min. The extract was dried under nitrogen stream at 40 ℃. The dried residue was dissolved in the mobile phase. Methyl tert-butyl ether 10.0 μL was then injected into HPLC for further analysis. Results The enrichment factor of diethylstilbestrol was 40. The method showed good linearity over the range of 7.814~97.670 μg/mL for diethylstilbestrol with r>0.999. The limit of detection were 2 μg/kg (S/N=3).The recoveries were 78.07%~88.46% with relative standard deviations of 0.99%~8.36%. Conclusion This method is sensitive, simple and suitable for determination of diethylstilbestrol in chicken.
标题：中空纤维膜液相微萃取-液相色谱法测定己烯雌酚
英文标题：Determination of diethylstilbestrol by hollow fiber-based liquid phase microextraction coupled with high pressure liquid chromatography
作者：
朱小红 陕西省食品药品检验所
盛喜霞 兵器工业卫生研究所
马鹏飞 陕西省食品药品检验所
惠卫甲 陕西省食品药品检验所
刘海静 陕西省食品药品检验所
中文关键词:中空纤维膜液相微萃取,液相色谱,己烯雌酚,鸡肉,
英文关键词:hollow fiber based liquid phase microextraction,high pressure liquid chromatography,diethylstilbestrol,chicken,
发表日期：2012-10-26
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