高效液相色谱-串联质谱法测定食品及保健品中维生素D的含量

目的建立食品及保健品中维生素D的含量测定方法。方法采用高效液相色谱-串联质谱法对食品及保健品中的维生素D含量进行测定。色谱柱为Waters ACQUITY UPLC BEH C₁₈柱(50.0 mm×2.1 mm,1.7μm),进样量5μL,柱温40℃,流速0.3 m L/min,流动相A为0.05%甲酸-5 mmoL甲酸铵溶液,流动相B为0.05%甲酸-5 mmo L甲酸铵-甲醇溶液,梯度洗脱;电离方式为电喷雾电离源正离子模式(ESI+),离子化电压5 500 V,鞘气和辅助气为氮气,传输管道温度550℃,鞘气流速35 L/min,碰撞气为氩气,喷雾气压力55 psi,采用动态多反应监测(MRM),正离子扫描。结果维生素D₂的回归方程为Y=508X-10 100,r=0.999 7,线性范围20～1 000μg/L;维生素D₃的回归方程为Y=415X-8 110,r=0.999 7,线性范围20～1 000μg/L。维生素D₂和维生素D₃的检出限均为2μg/kg,定量限均为5...

Content determination of vitamin D in food and health care products by high performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for content determination of vitamin D in food and health care products.Methods High performance liquid chromatography-tandem mass spectrometry( HPLC-MS) was used to determine the content of vitamin D in food and health care products.The column was Waters ACQUITY UPLC BEH C18 column( 50.0 mm×2.1 mm,1.7 μm),and the mobile phase was comprised of 0.05% formic-5 mmol ammonium formate solution A and 0.05% formic-5 mmol ammonium formate methanol solution B,by gradient elution method.The flow rate was 0.3 m L/min,the injection volume was 5 μL,and the column temperature was 40 ℃ .The ionization mode was the positive ion mode of the electrospray ionization source( ESI+),the ionization voltage was 5 500 V,the sheath gas and auxiliary gas were nitrogen,the temperature of the transmission pipe was 550 ℃,the velocity of sheath gas was 35 L/min,and the collision gas was argon. The pressure of the atomizer was 55 psi,and dynamic multi-reaction monitoring( MRM) and positive ion scanning were used.Results The regression equation of vitamin D2 was Y = 508 X-10 100,r = 0.999 7,with a linear range of 20 to 1 000 μg/L.The regression equation of vitamin D3 was Y = 415 X-8 110,r = 0.999 7,with a linear range of 20 to 1 000 μg/L. The detection limit was 2 μg/kg for D2 and D3,the quantitative limit was 5 μg/kg,relative standard deviation of precision( RSD) was 1.70% and 4.38%,respectively;the recovery rate was 3.71% and 2.90%,respectively. Conclusion This method is simple for preprocessing step and has high recovery rate,the accuracy and precision thereof can meet the actual testing needs,and it is suitable for the quantitative analysis and testing of vitamin D in food and health care products.