摘要
高效液相色谱串联质谱法是测定三聚氰胺公认的标准方法,具有灵敏度高、精密度好等特点。本研究对国家标准GB/T22388-2008中液相色谱串联质谱法进行了改进,对于液态奶、奶粉和鲜蛋基质,采用50%乙腈水溶液超声提取30min,提取液经过离心处理后,用Agela ASB-C18色谱柱(150×2.1mm,5μm)分离,乙腈和10mmol/L乙酸铵作为流动相(5∶95),用串联质谱在多反应监测模式下定量检测。方法定量限为0.01mg/kg,线性范围为0.01～0.5mg/L,相关系数r2>0.999,平均回收率为65%～80%,相对标准偏差为2.15%～6.68%(n=6)。
HPLC-MS/MS is a standard method with high sensitivity and precision for determination of melamine. Melamine was analyzed according to the method described by GB/T22388-2008 with the following modification. Melamine was extracted with aqueous 50% acetonitrile by ultrasonic treatment for 30min, and then centrifuged at 10000r/min for 10min.The supernatant was injected into a ASB-C18 column （ 150× 2.1mm,5μm,Agela）, using a mixture of acetonitrile and lOmmol/L ammonium acetate （5：95） as mobile phase at a flow rate of 0.2mL/min. Detection was performed by MS/MS in MRM mode.The limit of quantification （LOQ） was 0.01mg/L. The good linear was achieved from 0.01 to 0.5mg/L （r^2 〉0.999）.The recovery efficiency of method ranged between 65% and 80% ,and the relative standard deviation （RSD） were within 2.15%-6.68% （n =6）.
出处
《食品工业科技》
CAS
CSCD
北大核心
2009年第3期325-327,共3页
Science and Technology of Food Industry
