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当前位置: 首页 > 文章 > SA-UPLC-MS-MS联用测定奶粉中双氰胺的残留量 食品科学 2013,34 (18) 231-234
Position: Home > Articles > Determination of Dicyandiamide Residues in Milk by Syncore Analyst-Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry FOOD SCIENCE 2013,34 (18) 231-234

SA-UPLC-MS-MS联用测定奶粉中双氰胺的残留量

作  者：
张宪臣;王勇;张朋杰;华洪波;李云松;李蓉;李浩洋;杨芳;卢俊文
单  位：
中山出入境检验检疫局;中山市外语外贸大学附设外语学校
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
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线性关系良好(r>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。
译  名：
Determination of Dicyandiamide Residues in Milk by Syncore Analyst-Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry
作  者：
ZHANG Xian-chen;WANG Yong;ZHANG Peng-jie;HUA Hong-bo;LI Yun-song;LI Rong;LI Hao-yang;YANG Fang;LU Jun-wen;XIE Si-si;Zhongshan Entry-Exit Inspection and Quarantine Bureau;Zhongshan Foreign Language School Attached to Guangdong University of Foreign Studies;
关键词：
ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry(UPLC-MS-MS);;syncore analyst(SA);;dicyandiamide;;milk
摘  要：
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 cleaned up by hexane.The mass spectrometer was operated in the positive ion mode using select reaction monitoring for qualitative and quantitative analysis of dicyandiamide.The limit of detection(LOD) for dicyandiamide were 10 μg/kg,and limit of quantitation(LOQ) were 50 μg/kg.The correlation coefficient of the linear calibration curve was over 0.990 within the dicyandiamide concentration range 10–1000 ng/mL.The average recoveries for dicyandiamide were 99.6% to 102.3%(n = 6).The proposed method is simple,rapid,reliable,stable and sensitive.It can meet the requirements for the determination of dicyandiamide in milk.

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