摘要
建立了液相色谱-串联质谱法测定牛奶中4种内源雌激素的方法,可用于牛奶中17-α-雌二醇、17-β-雌二醇、雌三醇和雌酮等4种内源雌激素的同时测定。牛奶样品中添加内标化合物后,经过酶解、提取、净化、衍生等步骤获得上机试液,用LC-MS/MS测定,采用多反应监测正离子模式扫描。实验表明,4种化合物溶液质量浓度在0.0625-5.0μg/L之间有较好的线性关系,相关系数（R2）〉0.995,方法检出限在0.28-0.64 ng/kg之间。17-α-雌二醇回收率较低,只有60%左右,其它化合物的回收率均在72%-115%、相对标准偏差〈10%。在对57个样品的实际检测中,牛初乳E1,αE2,βE2,E3平均含量为3220,727,889,167 ng/kg;常乳中E1,αE2,βE2,E3含量为19.3-520 ng/kg,2.3-90.2 ng/kg,3.3-46.0 ng/kg,未检出-19.2 ng/kg。
A LC-MS/ MS method for determination of endogenous estrogens in milk has been developed. The 4endogenous estrogens were estrone（ E1）,17- α-estradiol（ αE2）,17- β-estradiol（ βE2） and estriol（ E3）. After adding the internal standards,the milk samples were processed by enzymolysis,extraction,purification and derivazation. And then the samples were measured by LC-MS/ MS. The technique allowed the determination of the proposed compounds in the concentration range from 0. 0625 μg/ L to 5. 0 μg/ L,within coefficient of linearity（ R2） higher than 0. 995. The experimental results showed the limits of detection from 0. 28 ng /kg to0. 64 ng/ kg. The recovery of α E2 was the lowest,only 60% or so. The recoveries of other compounds ranged from 72% to 115%,with relative standard deviations less than 10%. In 57 samples of actual testing,the average contents were found in bovine colostrum,with 3220,727,889,167 ng/ kg for E1,αE2,βE2and E3,respectively. And the contents in normal milk were 19. 3 - 520,2. 3 - 90. 2,3. 3 - 46 and not detected -19. 2 ng/ kg for E1,αE2,βE2and E3,respectively.
出处
《分析试验室》
CAS
CSCD
北大核心
2015年第7期751-755,共5页
Chinese Journal of Analysis Laboratory
基金
"十二五"农村领域国家科技计划项目(No.2011BAD26B0404)资助
