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HPLC-MS/MS法测定牛奶中两种玉米赤霉醇

     

摘要

玉米赤霉醇是一种违法的畜禽增重剂,国家明确将其列入非食用物质.针对牛奶样品前处理方法进行优化,采用高效液相色谱-三重四级杆串联质谱联用仪(HPLC-MS/MS)法测定牛奶中两种玉米赤霉醇的含量.样品直接采用乙腈提取,Waters MAX固相萃取小柱净化,负离子模式下,以乙腈-水为流动相进行梯度洗脱,以多反应监测(MRM)模式记录玉米赤霉醇的离子碎片响应进行定性定量分析.结果表明:采用优化后的提取方法、色谱条件及质谱条件,两种玉米赤霉醇的线性关系良好,线性范围为2.5 ng/mL~80.0 ng/mL,线性相关系数R2>0.999,α、β-玉米赤霉醇的平均回收率分别为108.5%和102.1%.该法简单、快捷,确证可靠,适用于牛奶基质样品中玉米赤霉醇类物质的检测.%Zeranol is one of the extender for livestock. It is included in the non edible substance list. A method for determination of zeranol in milk by HPLC-MS/MS was described. The samples were extracted with acetoni-trile, cleaned up with Waters MAX-SPE. After elution, the samples were analysed by MRM method in Negative mode. Acetonitrile-water was used as mobile phase and Ion fragment response was used to quantitative analysis. The linear range was 2.5 ng/mL-80.0 ng/mL, R2>0.999. Recoveries were 108.5%and 102.1%. The method is simple, rapid and reliable. It can be speculated that this method would be applied in the field of zeranol detec-tion in milk matrix.

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