超高效液相色谱质谱联用测定饲料牛乳及乳制品中双氰胺.PDF

19 2014, Vol.37 No.1 乳业科学与技术 ※分析检测 超高效液相色谱质谱联用测定饲料、 牛乳及乳制品中双氰胺 * 胡 雪，李翠枝 ，白艳梅，段国霞，赵 静，李慧秀 （内蒙古伊利实业集团股份有限公司，内蒙古 呼和浩特 0 10 110 ） 摘  要：建立超高效液相色谱质谱联用法检测饲料、牛乳及乳制品中双氰胺的方法。研究适用于检测饲料、牛乳及 乳制品的前处理方法，并对色谱柱进行了选择。样品经乙腈提取、C18 固相萃取填料净化后，低温冷冻离心除掉杂 质，含0.1% 甲酸的乙腈溶液和含0.1% 甲酸的10 mmol/L 甲酸铵水溶液梯度洗脱，通过Acquity BEH Amide色谱柱分 μg/L r 离，电喷雾正离子多反应监测模式进行检测。结果表明：该方法在1～1 000 范围内线性良好，相关系数 大于 0.995 ，饲料定量限最高40 μg/kg 。不同添加质量浓度的回收率为80.5%～108.4%，相对标准偏差小于7.0% 。该方法 具有简单方便、检测周期短，适用于饲料、牛乳及乳制品检测等特点。 关键词：超高效液相色谱质谱联用法；双氰胺；饲料；乳制品 Determination of Dicyandiamide in Feed, Milk and Dairy Products by UPLC-MS-MS HU Xue, LI Cui-zhi*, BAI Yan-mei, DUAN Guo-xia, ZHAO Jing, LI Hui-xiu (Inner Mongolia Yili Industrial Group Co. Ltd, Hohhot 0 10 110, China) Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for simultaneous determination of dicyandiamide in feed, milk and dairy products was developed. The extraction methods for feed, milk and dairy products were studied, and this was followed by selection of an appropriate chromatographic column. Samples were extracted with acetonitrile and the extract was then cleaned up on a C18 solid-phase extraction column, frozen and certrifuged to remove protein impurities, and separated on an Acquity BEH Amide column using a mobile phase composed of acetonitrile containing 0.1% formic acid and 10 mmol/L ammonium formate solution by gradient elution. Detection was performed by positive ion electrospray ionization (ESI) in multiple reaction