摘要
建立了牛奶、酸奶等奶制品中4种雌激素的分散固相萃取(DSPE)-液相色谱-质谱联用(LC-MS/MS)分析方法。样品中加入乙腈沉淀蛋白质,用无水MgSO4去除水分,再用N-丙基乙二胺(PSA)极性吸附剂分散固相萃取净化,液相色谱质谱联用测定,达到简单、快速、低成本和高回收率的目的。在优化条件下,该方法的检出限(S/N=3)为0.66~8.26μg/L。采用该方法测定了牛奶和酸奶中4种雌激素的含量,在三个水平下的加标回收率为78.99%~109.33%,相对标准偏差(RSD)为2.87%~9.23%。该方法可适用于牛奶、酸奶等乳制品中雌激素的检测。
method was developed for determining 4 estrogens in dairy products such as milk,yoghurt by dispersive solid phase extraction (DSPE) as clean up step and liquid chromatography-tandem quadrupole mass spectrometry(LC-MS/MS) as detection step. Acetonitrile was added into sample to precipitate the protein and anhydrous MgSO4 was used for the removal of residual water, and then sample was cleaned up by DSPE using primary secondary amine (PSA) dipolar adsorbent. Estrogens were detected by LC-MS/MS. This method could detect simple, quick and had low cost, high recovery. Under these optimized conditions,the limit of detection (S/N=3) ranged from 0.66μg/L to 8.26μg/L The average recovery of 4 estrogens from the milk and yoghurt samples at three spiked levels ranged from 78.99% to 109.33% with RSD of 2.87%-9.23%. The method could be used for the routine analysis of estrogens in milk and yoghurt as well as other dairy products.
出处
《食品工业科技》
CAS
CSCD
北大核心
2013年第6期53-56,60,共5页
Science and Technology of Food Industry
基金
"十二五"农村领域国家科技计划子课题(2011BAD09B0308)