婴儿配方乳粉中V_(A)、V_(D)和V_(E)混合标准物质的研制  

Preparation for mixed reference material of V_(A),V_(D) and V_(E) in infant formula milk powder

作　　者：宁霄[1] 金绍明[1] 刘彤彤 赵梅 曹进[1] NING Xiao;JIN Shaoming;LIU Tongtong;ZHAO Mei;CAO Jin(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《化学分析计量》2023年第7期1-6,共6页Chemical Analysis And Meterage

基　　金：国家重点研发计划高通量液质联用检测方法及诊断试剂研发(2021YFC2401100)。

摘　　要：研制婴儿配方乳粉中V_(A)、V_(D)和V_(E)混合标准物质。选择与日常检测水平相当的乳粉,经过混匀、分装、真空密封制备了候选标准物质。采用固相萃取-二维液相色谱建立了一种测定婴儿配方乳粉中V_(A)、V_(D)和V_(E)含量测定的通用方法,并将此法用于该标准物质的均匀性、稳定性检验及定值。定值采用同一检测方法8家实验室协作定值方式,并对标准物质的不确定度进行评估。采用该方法考察标准物质的均匀性和稳定性结果满足标准物质制备的要求。标准物质中V_(A)、V_(D)和V_(E)含量定值结果及其扩展不确定度(k=2)分别为(4987±3.1)μg/kg、(104±1.59)μg/kg和(90±1.3)mg/kg。该研究流程和结果符合标准物质定值的要求。该标准物质可用于相关检测实验分析方法的确认和过程质量控制。The reference material of V_(A),V_(D)and V_(E)in infant formula milk powder was prepared.The candidate reference materials were prepared by mixing,packaging and vacuum sealing of milk powder which was equivalent to the daily detection level.A general method for the determination of V_(A),V_(D)and V_(E)in infant formula milk powder was established by solid phase extraction column clean-up with two-dimensional liquid chromatography.The method was used to evaluate the homogeneity and stability of V_(A),V_(D)and V_(E)in the samples.The specified value was determined by using the same detection method in 8 laboratories,and the uncertainty of the reference material was evaluated.The results of homogeneity and stability of the samples by this method meet the requirements of reference material,and the specified values of V_(A),V_(D)and V_(E)(k=2)were(4987±3.1)μg/kg,(104±1.59)μg/kg,(90±1.3)mg/kg,respectively.The development process and the result conformed to the reference material fixed value requirement.This reference materials can be used in relevant detection experiments for the confirmation of V_(A),V_(D)and V_(E)analysis method.

关 键 词：脂溶性维生素 婴儿配方乳粉 标准物质 固相萃取-二维液相色谱 

分 类 号：O652.3[理学—分析化学]