当前位置: 首页 > 文章 > 鲜牛乳及乳制品中4种雌激素含量的HPLC测定 山东农业大学学报(自然科学版) 2015 (4) 519-523
Position: Home > Articles > Determination on 4 Estrogens Content in Fresh Milk and Dairy Products by HPLC Journal of Shandong Agricultural University(Natural Science Edition) 2015 (4) 519-523

鲜牛乳及乳制品中4种雌激素含量的HPLC测定

作  者:
谭欣同;邓立刚;赵善仓;董燕婕;王燕;李增梅
单  位:
山东农业科学院农业质量标准与检测技术研究所;山东农业大学食品科学与工程学院
关键词:
鲜牛乳;奶粉;雌激素;QuEChERS;HPLC
摘  要:
本文建立了鲜牛乳及奶粉中4种雌激素(17β-雌二醇、雌三醇、雌酮、己烯雌酚)的HPLC分析方法。奶粉样品溶解于水,Qu ECh ERS方法萃取,用乙腈沉淀蛋白质并提取雌激素,正己烷除脂,经氨基柱净化,C18色谱柱分离,采用紫外检测器,检测波长为230 nm。该方法对鲜牛乳及奶粉中17β-雌二醇、雌三醇、雌酮、己烯雌酚的检出限(S/N=3计)分别为0.03 mg/kg、0.026 mg/kg、0.03 mg/kg、0.012 mg/kg和0.024 mg/kg、0.021 mg/kg、0.025 mg/kg、0.01 mg/kg。定量限(以S/N=10计)分别为0.1 mg/kg、0.09 mg/kg、0.1 mg/kg、0.04 mg/kg和0.07 mg/kg、0.07 mg/kg、0.08 mg/kg、0.03 mg/kg在0.1、1.0、2.0 mg/kg三个浓度水平添加的平均回收率在81%~97%的范围内,RSD值在3.2%~8.7%之间。
译  名:
Determination on 4 Estrogens Content in Fresh Milk and Dairy Products by HPLC
作  者:
TAN Xin-tong;DENG Li-gang;ZHAO Shan-cang;DONG Yan-jie;WANG Yan;LI Zeng-mei;Collegeof Food Scienceand Engineering/Shandong Agricultural University;Instituteof Agricultural Quality Standardsand Testing Technology Research,Shandong Academyof Agricultural Sciences;Key Laboratoryof Test Technologyon Food Qualityand Safetyof Shandong Province;
关键词:
Fresh milk;;milk powder;;estrogen;;Qu ECh ERS;;HPLC
摘  要:
A novel method for the determination of 4 estrogens(17β-estradiol,Estriol,Estrone and Diethylstilbestrol)in raw milk and milk powder has been developed by HPLC. The milk powder was dissolved in water and then it was extracted with acetonitrile by Qu ECh ERS method and purified by NH2 solid phase extraction cartridge after fats were removed by hexane.The analyte was separated on a C18 column(Waters Atlantis d C18, 4.6 × 250 mm,i.d 5 μm) at UV 230 nm. The detection limits(S/N=3) of 17β-estradiol, estriol, estrone and diethylstilbestrol in milk powder and fresh milk were 0.03 mg/kg, 0.026mg/kg, 0.03 mg/kg, 0.012 mg/kg and 0.024 mg/kg, 0.021 mg/kg, 0.025 mg/kg, 0.01 mg/kg, respectively. The quantitation limit(S/N=10) in milk powder and raw milk were 0.1 mg/kg, 0.09 mg/kg, 0.1 mg/kg, 0.04 mg/kg and 0.07 mg/kg, 0.07 mg/kg,0.08 mg/kg, 0.03 mg/kg, respectively. The recoveries were 81%~97% with the range of RSD from 3.2% to 8.7%.

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