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建立了液相色谱-质谱联用法测定乳品中维生素D3质量浓度。试样经乙醇-50%氢氧化钾溶液皂化后,正己烷萃取,饱和氯化钠溶液净化,YMC C18色谱柱(50 mm×2.1 mm,3μm),甲醇-5 mmo L/L甲酸铵溶液作为流动相,梯度洗脱进行液相分离,采用电喷雾正离子方式,多反应选择离子监测,内标法峰面积定量。乳品中维生素D3质量浓度在0~50μg/L范围内线性良好,相关系数r均大于0.99,样品在20,100和200μg/kg三个质量浓度水平的添加平均回收率为83.9%~93.0%之间,变异系数为1.10%~4.90%(n=6),方法的定量限为20μg/kg。方法简便、准确,适用于婴幼儿食品和乳品中维生素D3的检测。
A liquid chromatography-mass spectrometry method was developed for the determination of vitamin D3 in dairy products. The sample was saponified by ethanol-50% potassium hydroxide solution, extracted with n-hexane and purified with saturated sodium chloride solution. The column was YMC C18 (50 mm × 2.1 mm, 3 μm) Mobile phase, gradient elution for liquid phase separation, using electrospray positive ion mode, multiple reaction selective ion monitoring, internal standard peak area quantitative. The linearity of the vitamin D3 in the range of 0 ~ 50μg / L was good and the correlation coefficient r was more than 0.99. The average recoveries of the samples at the three concentrations of 20, 100 and 200μg / kg were 83.9% ~ 93.0% The coefficient of variation was 1.10% ~ 4.90% (n = 6), and the limit of quantification was 20μg / kg. The method is simple and accurate, suitable for the detection of vitamin D3 in infant food and dairy products.