婴幼儿配方食品中维生素D_(3)检测方法比较研究  

Comparative Study on Detection Methods of Vitamin D_(3)in Infant Formula Foods

作　　者：周艳华[1] 李涛 卢岚[1] 李萍[1] ZHOU Yanhua;LI Tao;LU Lan;LI Ping(Changsha Environmental Protection College,Changsha 410004;Hunan Provincial Institute of Product and Goods Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410011)

机构地区：[1]长沙环境保护职业技术学院,长沙410004 [2]湖南省产商品质量检验研究院,食品安全监测与预警湖南省重点实验室,长沙410111

出　　处：《食品工业》2024年第1期319-323,共5页The Food Industry

基　　金：食品安全国家标准制修订项目(编号:spaq-2018-047)。

摘　　要：优化研究了婴幼儿配方食品中维生素D_(3)的超高效液相联用质谱法和液相色谱法。样本采用大样量稀释复溶,小样量批量快速前处理,对比研究超高效液相色谱联用质谱法和超高效液相色谱法等效性。超高效液相联用质谱法在20~400μg/L范围内,液相色谱法在50~1000μg/L范围内,均呈良好线性关系,相关系数R^(2)≥0.998。超高效液相联用质谱法定量限为0.879μg/100 g,低于液相色谱法定量限1.35μg/100 g。超高效液相联用质谱法加标回收率在88.0%~97.6%之间,相对标准偏差SRSD在4.8%~13.0%之间,液相色谱法加标回收率在89.8%~100.3%之间,相对标准偏差SRSD在2.0%~3.8%之间。优化后的检测方法样品代表性好,操作简单,可应用于所有类别婴幼儿配方食品,两种方法都具有等效性。The method of ultra-high performance liquid chromatography mass spectrometry and liquid chromatography for the determination of vitamin D3 in infant formula foods is optimized.Samples are diluted and redissolved in large quantities,while small quantities are quickly preprocessed in batches.There is a comparative study on the equivalence between ultra-high performance liquid chromatography coupled with mass spectrometry and ultra-high performance liquid chromatography.The Vitamin D3 shows a good linear relationship in the range of 20.0-400.0μg/L by LC-MS/MS,the Vitamin D_(3 )shows a good linear relationship in the range of 50.0-1000.0μg/L by HPLC,and the correlation coefficient R^(2) is more than 0.998.The limit of quantitation of LC-MS/MS method is 0.879μg/100 g,which is below the limit of quantitation of HPLC method(1.35μg/100 g).The recovery rate of Vitamin D3 by LC-MS/MS is in the range from 88.0%to 97.6%,with the precursorions(n=6)in the range of 4.8%to 3.0%,and the recovery rate of Vitamin D3 by HPLC is in the range from 89.8%to 100.3%,with the precursorions(n=6)in the range of 2.0%to 3.8%.The optimized detection method has good sample representativeness,simple operation,and can be applied to all categories of infant formula food.The two methods have equivalence.

关 键 词：婴幼儿配方食品 维生素D_(3) 方法等效性 前处理优化 

分 类 号：TS216[轻工技术与工程—粮食、油脂及植物蛋白工程]