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酶水解-高效液相色谱法测定肉类食品及牛奶中11种甾体激素 被引量:3

High Performance Liquid Chromatographic Determination of 11 Steroidal Hormones in Meat and Milk with Enzyme Hydrolysis of Sample
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摘要 碎肉用乙腈超声提取,挥干后加入KH2PO4缓冲液(牛奶直接加入KH2PO4缓冲液),再加β-葡萄糖醛酸酐酶,37℃恒温24 h,稀释后过SPE小柱,用乙腈洗脱,线性梯度变化的KH2PO4-CH3CN分离,二极管阵列检测器检测。所测11种激素的检出限为0.009-0.020 mg·kg^-1;平均回收率为51.0%-107.0%;相对标准偏差为0.77%-6.42%之间;相关系数为0.999 5-0.999 9之间。酶水解-高效液相色谱法测定肉类食品及牛奶中11种甾体激素是一种简便、快速、灵敏、线性好的检测方法。 Smashed meat sample was extracted ultrasonically with acetonitrile, and the extract was evaporated to dryness and taken up with phosphate buffer. Phosphate buffer was added directly to milk sample without pretreatment. Enzymehydrolysis was then performed by incubation at 37℃ for 24 h after the addition of glucuronidase. The hydrolyzed solution was filtered and passed through the SPE microcolumn, which was eluted with acetonitrile. One mL of the eluate was taken for HPLC separation and determination, using Zorbax Extend C18 as the stationary phase and the mixed solution of KH2PO4 and CH3CN as the mobile phase in the linear gradient elution. Detection limit, recovery and precision of the method for determination of 11 different steroidal hormones were tested, and values of results found were in the ranges 0. 009 - 0. 020 mg · kg^-1, 51.0% - 107. 0% and [RSD's (n=6)] 0. 77%-6.42% respectively.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2007年第6期482-484,487,共4页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金 2005年成都市卫生局课题(05018) 四川省医学重点实验室经费资助
关键词 高效液相色谱法 酶水解 甾体激素 肉类食品 牛奶 HPLC Enzyme-hydrolysis Steroidal hormones Meat Milk
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