婴幼儿乳粉中双氰胺的超高效液相色谱串联四极杆质谱法测定

Determination of dicyandiamide in infant milk powder by QuE ChE Rs- UPLC- MS / MS

应用超高效液相色谱串联四级杆质谱（UPLC-MS/MS）,建立了婴幼儿乳粉样品中双氰胺的分析方法。以水和乙腈作为基质的提取液,超声萃取基质中的双氰胺,沉淀蛋白,离心,上清液经PSA和C18进行净化,UPLC-MS/MS进行检测。Waters Acquity BEH Amide（1.7μm,3.0×100 mm）色谱柱分离,多反应监测模式,外标法定量,该物质在线性范围5～200 ng/m L内线性关系良好（R2〉0.99）。在市售乳粉基质中,对3个不同添加水平进行回收率考察,其回收率在80%～90%之间,相对标准偏差RSD（n=6）不大于11%。

An instrumental analytical approach has been developed for the rapid,fast detection of dicyandiamide by ultra-high pressure liquid chromatography coupled to tandem mass spectrometry（ UPLC-MS / MS）.Acetonitrile and water are used to extract dicyandiamide. The quick,easy,cheap,effective,rugged,safe（ Qu ECh ERs） sample preparation method was used to purify the dicyandiamide present in infant milk powder samples. The column of Waters Acquity BEH Amide（ 1. 7 μm,3. 0 × 100 mm） was used for separation,Multiple reaction monitoring mode and the external standard method were used for detection,and quantitative with the external standard method. The linear relationship is good（ R2 〉0. 99）. Three different spiked levels were studied in commercial infant milk powder. The recoveries are in the range of 80% ～ 90%,and the relative standard deviations（ RSDs,n = 6） are less than 17%.