超高效液相色谱法测定婴幼儿乳粉中维生素D_3质量分数  

Determination of cholecalciferol in infant formula milk powder by ultra performance liquid chromatography method

作　　者：樊垚[1] 任国谱[1] 王力清 綦艳 陈洪涛[3] 

机构地区：[1]中南林业科技大学,长沙410004 [2]广东产品质量监督检验研究院,广东佛山528300 [3]大连理工大学生命科学与技术学院,辽宁大连116024

出　　处：《中国乳品工业》2012年第12期44-47,共4页China Dairy Industry

基　　金：国家高技术发展计划(863计划)(2010AA23004);国家科技支撑计划(2012BAD12B04)

摘　　要：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。婴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0．1mL／min，柱温30℃，DAD扫波长范围190-400mm，检测波长为264nm，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0．2μg／100g。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。A fast,accurate and efficient ultra performance liquid chromatography （UPLC）method was developed for the determination of vita- min 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 p,g/100 g. This method demonstrated to be simple with high recovery and precision, and thus had a promising poten- tial for practical applications in cholecalciferol determination.

关 键 词：婴幼儿配方乳粉 维生素D3 超高效液相色谱 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]