高效液相色谱法测定乳粉中维生素E方法的优化

Optimization of the method for determination of vitamin E in milk powder by high performance liquid chromatography

中文关键词:  维生素E  异构体  高效液相色谱法  乳粉

英文关键词:vitamin E  isomer  milk powder  high performance liquid chromatography

中文摘要:

      目的 优化GB5009.82-2016 《食品安全国家标准 食品中维生素A、D、E的测定》中高效液相色谱法测定维生素E的样品制备和色谱分析条件。方法 样品经乙醇-氢氧化钾水浴皂化后, 石油醚-乙醚萃取, 氮吹至尽干, 甲醇溶解并过滤, 采用甲醇:四氢呋喃=99:1(V:V)作为流动相进行等度洗脱, 外标法定量。 结果 本方法在10 min内完成维生素E的4种异构体的分离分析, 精密度、线性良好。4种异构体在0.5、15和40 μg/mL添加水平的回收率为96.1%~101.2%, 维生素E的相对标准偏差小于1.7%(n=10), 方法定量限为100 μg/100g。结论 优化后的方法快速、准确、灵敏, 适合乳粉中维生素E异构体的快速准确测定。

英文摘要:

      Objective To optimize sample preparation and chromatographic analysis conditions of determination of vitamin E in milk powder by high performance liquid chromatography of GB 5009.82-2016 National food safety standard-Determination of vitamin A, D, E in food. Methods After the samples were saponified by ethanol potassium hydroxide bath, extracted by petroleum ether-ether, blown to dry by nitrogen, and dissolved with methanol, and then they were filtered. Methanol:tetrahydrofuran=99:1 (V:V) were used as the liquid phase, and external standard was used for quantitative determination. Results This method completed the separation and analysis of 4 isomers of vitamin E in 10 minutes with good precision and linearity. The recovery rates of 4 isomers at spiked levels of 0.5, 15 and 40 μg/mL were 96.1%-101.2%, the relative standard deviation of vitamin E was less than 1.7% (n=10), and the limit of quantitation was 100 μg/100 g. Conclusion The method is rapid, accurate and sensitive, which is suitable for the rapid and accurate determination of vitamin E isomers in milk powder.