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建立了婴幼儿配方乳粉中VB12的超高效液相色谱-串联质谱和超高效液相色谱测定方法。样品采用pH=4.0的醋酸钠溶液提取,经免疫亲和柱净化,采用Waters BEH C18色谱柱分离,液相法采用0.03 mol/L的磷酸缓冲盐(pH=3.5)和乙腈为流动相进行等度洗脱,紫外检测器波长为361 nm。质谱法以0.1%的甲酸水和甲醇为流动相进行梯度洗脱,采用电喷雾-正离子模式多反应监测进行定性和定量分析,外标法定量。VB12在10~500μg/L的质量浓度范围内线性关系良好,VB12的检出限均为0.5μg/kg,定量限均为1.5μg/kg,液相方法回收率为90.2%~98.3%,相对标准偏差为1.4%~2.5%,液相色谱-质谱法回收率为89.3%~95.7%,精密度在1.9%~3.1%。该方法简单、灵敏度高、分析时间短、定量准确,适用于婴儿乳粉中VB12的测定。
The establishment of infant formula milk powder VB12 ultra performance liquid chromatography - tandem mass spectrometry and ultra performance liquid chromatography determination. The samples were extracted with sodium acetate solution (pH = 4.0), purified by immunoaffinity column and separated on a Waters BEH C18 column. The mobile phase consisted of 0.03 mol / L phosphate buffer (pH = 3.5) and acetonitrile Degree of elution, UV detector wavelength of 361 nm. Mass spectrometry was performed with gradient elution with 0.1% formic acid in water and methanol as the mobile phase. Qualitative and quantitative analysis was carried out by electrospray - positive ion mode multi-reaction monitoring. The linearity of VB12 was in the range of 10 ~ 500μg / L. The detection limit of VB12 was 0.5μg / kg, the limit of quantitation was 1.5μg / kg, and the recovery of liquid phase method was 90.2% ~ 98.3% The standard deviation was 1.4% ~ 2.5%. The recovery of liquid chromatography-mass spectrometry was 89.3% ~ 95.7% with the precision of 1.9% ~ 3.1%. The method is simple, high sensitivity, short analysis time, quantitative accuracy, suitable for the determination of infant milk powder VB12.