超高效液相色谱法测定乳及乳制品中维生素D的含量
目的 建立用正相高效液相色谱硅胶柱净化维生素D, 通过反相超高效液相色谱测定乳及乳制品中维生素D的含量的一种快速检测方法。方法 样品经氢氧化?–钾皂化后, 用石油醚萃取, 萃取液经无水硫酸钠脱水、旋蒸, 定容, 用正向色谱净化, 反相超高效液相色谱用以0.1 mL/min流速的甲醇/水(97:3V:V)为流动相, 采用WatersACQUITY UPLC BEH C18色谱柱分离, 紫外检测器检测, 内标法定量。结果 维生素D3浓度在0.05–1.00 μg/mL内标准曲线相关系数(r2)均大于0.995。在质量分数为0.5、1.0、2.0 μg/mL 3个加标水平下, 加标回收率为65.0–115.0%, 相对标准偏差为0.1%–1.4%。结论该方法简便、快速、实用、准确,各项技术指标满足标准的要求,可用于乳及乳制品中维生素D的定量检测。
Objective To establish a rapid method for the determination of vitamin D in milk and dairy products by reversed phase–ultra performance liquid chromatography (RP-UPLC) after normal phase–high performance liquid chromatography (NP-HPLC) with silica gel column purification. Methods Samples were saponified by potassium hydroxide and extracted with petroleum ether, then the extract liquor was dehydrated by anhydrous sodium sulfate, rotary evaporated and fixed volume. NP-HPLC was used to purify and for RP-UHPLC, methanol/water (97:3 V:V) at 0.1 mL/min flow rate served as mobile phase,WatersACQUITY UPLC C18 chromatographic column was used for separation, and UV detector and quantitative internal standard method were used for vitamin D determination. Results Relation coefficient (r2) of the internal standard curve was greater than 0.995 in the range of vitamin D3 concentration of 0.05–1.00 μg/mL. The recovery rate was 65.0%–115.0% and the relative standard deviation was 0.1%–1.4% when the mass fraction was 0.5, 1.0 and 2.0 μg/mL. Conclusion This method is simple, rapid, practical and accurate, and can be used for the quantitative determination of vitamin D in milk and dairy products.
标题：超高效液相色谱法测定乳及乳制品中维生素D的含量
英文标题：Determination of vitamin D in milk and dairy products by ultraperformance liquid chromatography
作者：
施鹏飞 淮南益益营养食品科技有限公司
王晓薇 淮南益益营养食品科技有限公司
王巧云 淮南益益营养食品科技有限公司
李光辉 淮南益益营养食品科技有限公司
马镇 淮南益益营养食品科技有限公司
中文关键词:乳制品,维生素D,正相净化,超高效液相色谱法,
英文关键词:dairy products,vitamin D,positive phase purification,ultra performance liquid chromatography,
发表日期：2019-11-12
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