摘要
对不同牛奶中雌三醇的含量进行分析,探索建立HPLC法快速测定牛奶中雌三醇含量的方法。样品经乙腈处理沉淀蛋白质,正已烷脱脂净化后,取上清液浓缩,采用反相高效液相色谱法,流动相为乙腈+甲醇+四氢呋喃+醋酸钠溶液(0.01moL/L)=20+20+10+50(V/V),Agilent-Cl8柱(4.6mm×300mm,5um),流速为1.0mL·min-1,波长为230nm,进样量20μL,雌三醇浓度在(0.1×10-6～2.0×10-6)g/mL时,浓度与峰面积呈线性关系,加标回收率为92.50%～103.9%,最低检出限为0.08ng/mL,定量限0.27ng/mL,相对标准偏差为2.04%～7.76%。
The concentrations of estriol in different milk were analyzed,in order to establish a rapid method by HPLC to determine the estriol concentrations in milk.The proteins of samples were deposited by acetonitrile and the fats were removed by hexane and then the supernatant liquor concentrations were detected by RP-HPLC method.The chromatographic conditions included Agilent-Cl8 column（4.6mm×300mm,5 um） and the mobile phase consisting of a mixture of acetonitrile,methanol,tetrahydrofuran and 0.01 mol/L of sodium acetate solution by 20：20：10：50 （V/V）. The flow rate was 1.0 mL/min. Detection wavelength was at 230 nm. The sample dose was 20 μL. When the concentration of estriol was at 0.1 × 10^-6 g/mL to 2.0× 10^-6 g/mL, the perfect linearity between concentration and peak area ratio was obtained. The recovery rate was 92.50% to 103.9%. The detection limit was 0.08 ng/mL and the quantificational limit was 0.27 ng/mL. The relative standard deviation （RSD） was 2.04% to 7.76%.
出处
《食品工业》
北大核心
2009年第5期61-63,共3页
The Food Industry
