摘要
目的:建立超高效液相色谱-电喷雾串联四极杆质谱(UPLC-ESI-MS/MS)快速测定原料乳和乳制品中三聚氰胺的方法。方法:样品经Oasis MCX柱净化,超高速离心,采用UPLC-ESI-MS/MS、正离子方式、多离子反应监测(MRM)定量法检测三聚氰胺。结果:经方法学验证,该方法对三聚氰胺的最低检出浓度为1.0μg/kg(进样量10μl),最低检测浓度为5.0μg/kg。在0.5~100.0μg/L的线性范围中,相关系数r〉0.9995,回收率:89%~104%。结论:方法灵敏度高、操作简单、定量准确、测定浓度范围宽阔,是原料乳和乳制品中三聚氰胺含量检测的理想方法。
Objective:A UPLC-ESI-MS/MS method was developed for the determination of melamine in raw milk and dairy products.Methods: Sample was extracted and purified by SPE Oasis MCX.After centrifugation,melamine was determined by UPLC-ESI(+)-MS/MS and quantified with multiple reaction monitoring(MRM) mode.Results: The detection limit(LOD) for melamine was 1.0 μg/kg.The limit of quantification(LOQ) was 5.0 μg/kg.The linear range was from 0.5 to 100 μg/L with correlation coefficients above 0.9995.The mean recoveries were between 89% and 104%.Conclusion: This method can be applied for the determination of melamine in raw milk and dairy products for its high sensitivity and high selectivity.
出处
《中国卫生检验杂志》
CAS
2010年第9期2184-2186,共3页
Chinese Journal of Health Laboratory Technology