SA-UPLC-MS-MS联用测定奶粉中双氰胺的残留量-河南农业科学.PDF

※分析检测 食品科学 2013, Vol.34, No.18 231 SA-UPLC-MS-MS联用测定奶粉中 双氰胺的残留量 1 1 1 2 1,* 1 1 1 1 1 张宪臣 ，王 勇，张朋杰，华洪波，李云松 ，李 蓉 ，李浩洋，杨 芳 ，卢俊文，谢思思 (1.中山出入境检验检疫局，广东 中山  528403 ；2. 中山市外语外贸大学附设外语学校，广东 中山  528401) 摘  要：建立超高效液相色谱- 串联质谱(UPLC-MS-MS)检测奶粉中双氰胺残留量的检测方法。以氘代试剂为内 标，样品经氨化乙腈萃取后，平行定量浓缩仪浓缩，用正己烷脱脂，采用UPLC-MS-MS选择反应监测(SRM)正离子 模式测定。双氰胺的检出限可达10µg/kg，最低定量限可达50µg/kg 。在10～1000ng/mL范围内峰强度与质量浓度的 r 线性关系良好( ＞0.990) 。方法的平均回收率在99.6%～102.3%之间。方法简单、快速、稳定、准确、灵敏度高，能 够满足日常工作中奶粉双氰胺的检测要求。 关键词：超高效液相色谱- 串联质谱；平行定量浓缩仪；双氰胺；奶粉 Determination of Dicyandiamide Residues in Milk by Syncore Analyst-Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry 1 1 1 2 1,* 1 ZHANG Xian-chen ，WANG Yong ，ZHANG Peng-jie ， HUA Hong-bo ，LI Yun-song ，LI Rong ， 1 1 1 1 LI Hao-yang ，YANG Fang ，LU Jun-wen ，XIE Si-si (1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China； 2. Zhongshan Foreign Language School Attached to Guangdong University of Foreign Studies, Zhongshan 528401, China) Abstract ：A method for the determination of dicyandiamide in milk was developed by syncore analyst/ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (SA-UPLC-MS-MS). Deuterium substituted reagents were used as internal standards and added to the sample before extraction. The mixture was extracted with aminated acetonitrile, concentrated with syncore analyst, and cle