超高效液相色谱-串联质谱法测定食品中维生素D

Determination of Vitamin D in Foodstuffs by UPLC-MS/MS

[目的]建立超高效液相色谱-串联质谱测定食品中维生素D含量的分析方法。[方法]样品经氢氧化钾-乙醇溶液皂化、正己烷萃取、浓缩后,采用Agilent XDB-C 18色谱柱分离、10 mmol/L甲酸铵甲醇-水溶液等度洗脱,经电喷雾正离子多反应监测模式进行检测,内标法定量。[结果]维生素D 2和D 3在5~500 ng/mL线性关系良好,二者检出限为2μg/kg,定量限为5μg/kg。在各浓度水平下,二者的回收率为83.1%~105.4%,RSD为4.3%~8.7%。[结论]该方法准确性好、灵敏度高,适用于食品中维生素D的分析测定。

[Objective]To establish an analytical method for the determination of vitamin D in foodstuffs by ultra-high performance liquid chromatography tandem quadrupole mass spectrometry method.[Method]The sample was saponified by potassium hydroxide-ethanol solution and extracted by n-hexane,after being concentrated,the analytes were separated on Agilent XDB-C18 column,eluted by the mobile phase consisted of ammonium formate methanol solution and water and identified by ESI-MRM,meanwhile,quantitated by internal standard method.[Result]Vitamin D2 and D3 had a linear relationship between 5 and 500 ng/mL.The detection limit(LOD)was 2μg/kg,and the limit of quantification(LOQ)was 5μg/kg.The recoveries ranged from 83.1%to 105.4%,RSD was 4.3%-8.7%.[Conclusion]The method has good accuracy and high sensitivity,and is suitable for the analysis and determination of vitamin D in foodstuffs.