作　　者： ; ; ; ; ; ; ; ;

机构地区： 中国广州分析测试中心

出　　处： 《分析测试学报》 2013年第3期271-274,共4页

摘　　要： 建立了奶粉中双氰胺的高效液相色谱-串联质谱快速测定方法。实验优化了前处理条件、液相色谱条件和质谱参数。样品经水提取,乙腈分次沉淀蛋白后,采用亲水高效液相色谱柱分离,流动相为乙腈(含0.2%甲酸)-0.1%甲酸(含10 mmol/L甲酸铵)(体积比95∶5),流速0.3 mL/min。采用正离子模式的电喷雾质谱检测,多反应(MRM)选择离子监测,检测离子对为m/z 85→68和m/z 85→43,检测周期为5 min。结果显示,双氰胺在0.2～100μg/L范围内线性良好,相关系数为0.999 8。双氰胺的检出限为0.1μg/L,方法的定量下限为5μg/kg。低、中、高3个加标水平下的平均回收率为79%～83%,相对标准偏差为2.7%～6.5%。方法简便快速、准确可靠,已用于奶粉中双氰胺的检测。 A method was developed for the determination of dicyandiamide in infant milk powder by high-performance liquid chromatography - mass spectrometry （ LC - MS/MS）. The conditions of ex- traction and parameters of LC -MS were optimized. The sample was extracted with water, precipita- ted with acetonitrile, then separated on a Thermo syncronis column using mixture of acetonitrile （ containing 0. 2% formic acid） -0.1% formic acid（containing 10 mmol/L ammonium formate） （95 ： 5） as mobile phase at a flow rate of 0. 3 mL/min. The detection of dicyandiamide was performed by posi- tive-ion electrospray ionization mass spectrometry（ ESI- MS） utilizing multiple reaction monitoring two parent- daughter ion pairs： m/z 85/68 and 85/43. A good linear relationship was obtained in the range ofO. 2-100 μg/L, with a correlation coefficient of 0. 999 8. The spiked recoveries at dif- ferent spiked levels were in the range of 79% -83% . The detection limit of dicyandiamide was 0.1μg/L, and the quantitatiion limit of method was 5 μg/kg. The results indicated that the method was rapid, selective, sensitive and stable enough to examine dicvandiamide in infant milk powder.

关 键 词： 双氰胺 液相色谱 串联质谱 奶粉

领　　域： [理学] [理学] [理学] [理学]