A fast、accurate and efficient ultra performance liquid chromatography (UPLC) method was developed for the determination of vitamin D3 in infant milk powder. Infant formula milk powder was extracted by petroleum ether after saponification together with lipase,ascorbic acid - ethanol solution and KOH solution at a low temperature. The residue was dissolved in methanol and finally injected into the UPLC system after the extraction solution was evaporated to?dry under a rotary evaporator. The chromatographic separation was performed at 30℃ in the isocratic elution mode using a mobile phase composed of a mixture of methanol and water (97:3,V/V) at the flow of 0.1mL/min under the detective wavelength of 264 nm.The cholecalciferol was finally quantified by external standard method.Results: The average spike recoveries of 3 replicates were at 3 levels of 93.4% 、95.3% and 96.5% with the relative standard deviations (RSD)of 1.45%. The detection limit of cholecalciferol was 0.2 μg /100 g. This method demonstrated to be simple with high recovery and precision, and thus had a promising potential for practical applications in cholecalciferol determination.%针对婴幼儿配方乳粉中维生素D3的测定,开发出一种快速、准确、高效的超高效液相色谱方法.耍幼儿配方乳粉经脂肪酶、抗坏血酸-乙醇溶液和KOH溶液低温皂化后石油醚萃取,萃取液经旋转蒸发,最终用甲醇定容后,用超高效液相色谱仪检测.以甲醇+水为流动相等度洗脱,流速0.1 mL/min,柱温30 ℃,DAD扫描波长范围190~400 nm,检测波长为264 nm,维生素D3外标法定量.结果表明:维生素D3加标回收率为93.4%,95.3%和96.5%,RSD为1.45%,最低检出限为0.2 μg/100 g.本法操作步骤简单、回收率及精密度较高,适用于婴幼儿配方乳粉及同类产品中维生素D3的快速测定.
展开▼