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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 被引量:1

Determination of melamine residue in ultra by performance liquid chromatography tandem mass spectrometry
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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.
出处 《中国蜂业》 2011年第Z2期42-45,共4页 Apiculture of China
关键词 SPE UPLC-MEC-MS-MS 内标 三聚氰胺 蜂蜜 SPE UPLC-MEC-MS-MS internal standard melamine honey
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