超高效液相色谱-质谱联用测定维生素预混合饲料中生物素含量

Determination of biotin in premix feed with UPLC-MS/MS

建立了维生素预混合饲料中生物素含量的超高效液相色谱质谱联用测定方法。样品用水提取后以Acquity UPLC BEH C18柱(2.1×50mm,1.7μm)为色谱柱分离,以电喷雾电离串联质谱在正离子选择反应监测(SRM)模式下进行测定。以V(乙腈)∶V(0.1%甲酸)=15∶85为流动相,流速为0.2mL/min,色谱柱温度为40℃,进样量为2μL;定量子离子为227.1,定性子离子为227.1、97.1、123.0,二级碰撞室内对应的碰撞能量分别为:11、22、37V。对空白试样进行3个浓度水平4个重复的添加试验。结果表明:回收率78.2%～93.2%,相对标准偏差1.5%～2.8%。该方法检测限0.2mg/kg,线性范围0.010～5.000μg/mL。

A method for the determination of biotin in premix feed by UPLC-MS /MS is described. The sample was extracted with water,and then analyzed using UPLC-MS/MS in selective reaction monitoring (SRM) mode via positive electrospray ionization with an Acquity UPLC BEH C18 column (2.1×50 mm,1.7 μm) as the analytical column. Mobile phase are acetonitrile and 0.1% formic acid (15:85,by volume) and injection volume is 2 μL,at a flow rate of 0.2 mL/min. Column temperature is 40 ℃. Quantitative product ion is m/z 227.1,...