建立了婴幼儿配方奶粉中维生素D的液相色谱-大气压化学电离串联质谱(LC-APCI-MS/MS)分析方法.样品经正己烷和甲基叔丁基醚混合溶液提取,ProElut VDC固相萃取柱净化,Kinetex C18色谱柱分离,采用大气压化学电离(APCI)源、正离子扫描和多反应监测(MRM)模式对维生素D2和维生素D3进行检测,内标法定量.结果表明维生素D2和维生素D3在5~5000 μg/L范围内均具有良好的线性关系,检出限为2 μg/kg,定量限为5 μg/kg.在5、10和100 μg/kg添加水平下,维生素D2和维生素D3的回收率为85.2%~105.3%,相对标准偏差为4.7%~8.1%.该方法简便准确,灵敏度高,适用于婴幼儿奶粉中维生素D的测定.
A method using liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI-MS/MS) was developed for the determination of vitamin D in infant formula.The milk powder sample was extracted with hexane and tert-butyl methyl ether followed by clean-up with ProElut VDC cartridge.The LC separation was performed on Kinetex C18 column (100 mm×4.6 mm, 2.6 μm) by a gradient elution using water and acetonitrile as the mobile phases with a flow rate of 1.0 mL/min.Identification of vitamin D2 and vitamin D3 was achieved by APCI-MS/MS using multiple reaction monitoring (MRM).The quantification analysis was performed by internal standard method.The calibration curves showed a good linearity in the range of 5-5000 μg/L.The limits of detection (LODs) for vitamin D2 and vitamin D3 in the formula were 2 μg/kg.The limits of quantification (LOQs) for vitamin D2 and vitamin D3 in the formula were 5 μg/kg.The average recoveries of vitamin D from milk powder spiked at 5, 10 and 100 μg/kg levels were between 85.2% and 105.3%, and the relative standard deviations were between 4.7% and 8.1%.The simple, accurate and sensitive method is suitable for the determination of vitamin D in infant formula.
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