超声萃取-高效液相色谱法同时测定奶粉中4种雌激素类残留.PDFVIP

156 2014, Vol.35, No.12 食品科学 ※分析检测 超声萃取-高效液相色谱法同时测定奶粉中 4 种雌激素类残留 谭 芳，黄 璐，郑 琦* （江汉大学光电化学材料与器件省部共建教育部重点实验室，湖北 武汉 430056 ） 摘  要： - 建立超声波萃取 高效液相色谱法同时测定奶粉中炔雌醇、己烯雌酚、壬基酚、苯甲酸雌二醇残留量的方 法。样品以乙腈超声萃取、离心，提取液浓缩后经0.45 μm滤膜过滤，进高效液相色谱仪分析。研究萃取溶剂、萃取 时间及离心时间对萃取效率的影响，确立色谱检测条件。结果表明，乙腈和0.043 mol/L磷酸二氢钠缓冲液（用磷酸 pH 5 1 mL/min 30 224 nm 3 20 μg/kg 调至 值到 ）为流动相，梯度洗脱，流速 ，柱温 ℃，检测波长 。方法的检出限为 ～ ， 4 种组分得到良好分离，加标回收率在80.2%～101.0%之间，工作曲线的相关系数在0.992 4～0.999 7之间，相对标 准偏差在0.95%～2.04%之间（n=3 ），方法快速、灵敏度高、分离效果好，样品处理简单、无杂质干扰，能够满足 奶粉中雌激素分析的需要。 关键词：超声波萃取；高效液相色谱法；奶粉；雌激素 Simultaneous Determination of Four Estrogen Residues in Powdered Milk Using Ultrasonic Extraction-HPLC * TAN Fang, HUANG Lu, ZHENG Qi (Key Laboratory of Optoelectronic Chemical Materials and Devices, Ministry of Education, Jianghan University, Wuhan 430056, China) Abstract: A method was developed for the simultaneous determination of residues of ethinyl estradiol, diethylstilbestrol, 4-nonylphenol and estradiol benzoate in powdered milk by high performance liquid chromatograph (HPLC) after ultrasonic extraction. Samples were ultrasonically extracted with acetonitrile and after centrifugation of the extract, the supernatant was concentrated and filtrated through a 0.45 μm filter before analysis by HPLC. Extraction solvent, extraction and centrifugation time, and HPLC conditions were optimized. The analysis was conducted by using gradient elution with acetonitrile-0.043 mol/L NaH PO buffer as the mobile phase. Unde