液相色谱-质谱联用法同时测定保健食品中维生素D3和维生素K1的含量

Simultaneous determination of thevitamin D and vitamin K content in healthy foodby liquid chromatography mass spectrometry

目的建立液相色谱-质谱联用法同时测定维生素D3和维生素K1的含量。方法样品经前处理,于液相色谱-质谱联用仪中进行检测,采用5mmol/L甲酸铵甲醇溶液为流动相,等度洗脱,经C18色谱柱(4.6mm×150mm,2.6μm)分离。结果维生素D3在浓度0.0546~0.819μg/mL之间呈现良好的线性关系,r=0.9990,平均回收率为92.15%~98.99%,RSD为2.4%;在0.134~2.006μg/mL之间,维生素K1的浓度,呈现良好的线性关系,r=0.9990,平均回收率为94.15%~101.01%,RSD为2.2%。结论该方法能同时测定维生素D3和维生素K1含量,操作简便准确、耗费时间短、重现性较好,可在实验室广泛推广。

Objective To establish a method for the simultaneous determination of vitamin D3 and vitamin K1 content by liquid chromatography mass spectrometry. Methods The samples were pretreated and detected by liquid chromatography-mass spectrometry. The 5 mmol/L ammonium formate and methanol were used as mobile phase for isocratic elution,and the sample was separated by C18 column(4.6 mm×150 mm,2.6 μm). Results Vitamin D3 had a good linear relationship in range of 0.0546-0.819 μg/mL(r=0.9990),the recoveries were 92.15%-98.99%,and the RSD was 2.4%.Vitamin K1 had a good linear relationship in range of 0.134-2.006 μg/mL(r=0.9990),the recoveries were 94.15%-101.01%,and the RSD was 2.2%. Conclusion This method can simultaneously determine the vitamin D3 and vitamin K1 content in healthy food,which is simple,accurate,time-consuming and reproducible,and can be widely used in laboratory.