固相萃取-超高压液相色谱-电喷雾串联质谱法测定蜂蜜中的三聚氰胺  

Determination of melamine residue in ultra by performance liquid chromatography tandem mass spectrometry

作　　者：王飞[1] 曹彦忠[1] 李学民[1] 贾光群[1] 刘晓茂[1] 

机构地区：[1]河北秦皇岛出入境检验检疫局,秦皇岛066002

出　　处：《中国蜂业》2011年第Z2期42-45,共4页Apiculture of China

摘　　要：用5%三氯乙酸溶液溶解三聚氰胺、去除蜂蜜中的蛋白质干扰,经MCX固相萃取柱分离后,UPLC/MEC-MS-MS检测,内标法定量。在10.0～200μg/kg范围内线性关系良好,r=0.9999。检出限(LOD)为5.0μg/kg,定量限(LOQ)为10.0μg/kg。在线性范围内的添加水平的平均回收率为84.4%～115.0%,相对标准偏差≤6.6%。方法有良好的精密度和重现性,适用于蜂蜜中的三聚氰胺检测。A method for fast determination melamine residue in honey was established,by using ultra performance liquid chromatography coupled with electrospray tandem mass spectrometry with electrospray ionization quadrupole tandem mass spectrometry(UPLC-ES-MS/MS).Internal standard quantitative.The residue was quantified with multiple reaction monitoring(MRM)mode.The method was validated and good results were obtained with respect to precision,repeatability and spiked recovery.The limit of detection was 5μg/kg for melamine,limit of quantitation 10μg/kg,and the linear range was Ranged from 10 to 200μg/kg,The average recoveries were between 84.4%～115.0%in the spiked range of 10～200μg/kg,and the relative standard deviations(RSDs) were between≤6.6%.The method has good repeatability and high sensitivity,and can be applied for the determination of melamine residue in honey.

关 键 词：SPE UPLC-MEC-MS-MS 内标 三聚氰胺 蜂蜜 

分 类 号：S896.8[农业科学—特种经济动物饲养]