超高效液相色谱-串联质谱法测定牛奶中重组牛生长激素 N-末端肽链

摘要

UHPLC-MS/MS was applied to the determination of N-terminal peptide of recombinant bovine somatotropin in milk.The sample solution was diluted to constant volume with the mixture of acetonitrile and 0.05% (φ)formic acid solution (4+6).Waters ACQUITY BEH-C18 column was used as stationary phase,and the mixture of acetonitrile and 0.05% (φ)formic acid solution mixed in different ratio was used as mobile phase in gradient elution.ESI+ and multi-reactions monitor were adopted in MS/MS.Linear relationship between values of peak area and mass concentration of N-terminal peptide of recombinant bovine somatotropin was obtained in the range of 0.1-2 mg·L-1 ,with lower limits of determination(10S/N)of 0.02 mg·kg-1 .On the base of blank milk sample,test for recovery was made by standard addition method;values of recovery found were in the range of 85.0%-88.6%,with RSD′s (n=6)less than 9%.%建立了高效液相色谱-串联质谱法测定牛奶中重组牛生长激素 N-末端肽链的方法。样品溶液以乙腈-0．05％（体积分数）甲酸（4＋6）溶液作为定容溶剂。以 Waters ACQUITY BEH-C18色谱柱为分离柱，以不同体积比的乙腈和0．05％甲酸溶液混合液为流动相进行梯度洗脱，采用电喷雾正离子源多反应监测模式检测。重组牛生长激素 N-末端肽链的质量浓度在0．1～2 mg·L-1范围内与其峰面积呈线性关系，测定下限（10S/N）为0．02 mg·kg-1。以空白牛奶样品为基体进行加标回收试验，所得回收率在85．0％～88．6％之间，测定值的相对标准偏差（n＝6）小于9％。