作　　者： ; ; ; ; ; ; ; ;

机构地区： 中国广州分析测试中心

出　　处： 《分析测试学报》 2008年第10期1044-1048,共5页

摘　　要： 摘采用气相色谱-质谱（GC-MS）分析技术，选择离子检测法（SIM），开发出一种准确可靠、灵敏度高的测定奶粉及奶制品中三聚氰胺的新方法。色谱柱为DB-1 Ms石英毛细管柱，进样口温度280℃，柱温75℃，保持1min，再以30℃／min升至290℃。载气He，流量1．0mL／min。EI离子源，选择m／z 171、285、327、342用于SIM检测，根据这4个离子的抽出离子色谱图的峰面积比进行目标物确证，以基峰m／z 327做定量分析。三聚氰胺的线性范围为0．01～50mg／L，平均回收率为90％～98％，检出限为1μg／kg，定量下限为5μg/kg。该法与现有方法相比灵敏度提高了2个数量级，用色谱保留时间、质谱同时定性，消除了奶粉及奶制品中杂质的干扰，避免了可能产生的假阳性，结果准确可靠，选择性和重复性好，适用于奶粉及奶制品的检验。 A new method for determination of melamine in milk powder and milk products by gas chromatography-mass spectrum with selected ion monitor（ GC -MS/SIM） was established in this paper. The conditions for GC - MS were optimized, and the ions selected were m/z 171, 285, 327, 342. Qualitative assessment was acquired by the four characteristic ions and retention time, and quantitative assertion was achieved using base peak m/z 327. The linear range was 0.01-50 mg/L, and the average recovery for melamine was in the range of 90%-98% with detection limit as low as 1 μg·kg^-1. The sensitivity for this method was two orders of magnitudes higher than the presently existed method. The qualitative assessment was conducted using both retention time and mass spectrum to avoid the matrix effect in milk powder and milk products. The method has been applied to the determination of melamine in milk powder and milk products with satisfactory results.

关 键 词： 三聚氰胺 奶粉 奶制品 气相色谱 质谱 选择离子检测

领　　域： [理学] [理学] [轻工技术与工程] [轻工技术与工程]