食品与发酵工业 >

2023 , Vol. 49 >Issue 4: 268 - 273

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.030970

分析与检测

在线固相萃取/二维液相色谱法同时测定婴幼儿配方奶粉中多种脂溶性维生素

  • 毛燕妮 ,
  • 许晴 ,
  • 李宏铨 ,
  • 聂懿 ,
  • 朱静璇 ,
  • 柳慧冰 ,
  • 康翠欣
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  • 1(武汉食品化妆品检验所,湖北 武汉,430040)
    2(国家市场监管重点实验室(食用油质量与安全),湖北 武汉,430040)
硕士,工程师(康翠欣高级工程师为通信作者,E-mail:281806656@qq.com)

收稿日期: 2022-01-31

  修回日期: 2022-03-31

  网络出版日期: 2023-03-20

基金资助

湖北省市场监督管理局技术保障专项项目(Hbscjg-JS202006)

收起

Simultaneous determination of fat-soluble vitamins in infant formula by online solid phase extraction with two-dimensional liquid chromatography

  • MAO Yanni ,
  • XU Qing ,
  • LI Hongquan ,
  • NIE Yi ,
  • ZHU Jingxuan ,
  • LIU Huibing ,
  • KANG Cuixin
Expand
  • 1(Wuhan Institute for Food and Cosmetic control, Wuhan 430040, China)
    2(Key Laboratory of National Market Supervision (Edible Oil Quality and Safety), Wuhan 430040, China)

Received date: 2022-01-31

  Revised date: 2022-03-31

  Online published: 2023-03-20

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摘要

利用在线固相萃取技术结合二维液相色谱仪,建立婴幼儿配方奶粉中维生素A、D、E、K1同时测定的方法。将奶粉样品皂化后,利用PLRP-S聚合物为填料的在线固相萃取柱净化强碱性皂化液,以五氟苯基柱为一维色谱柱,在紫外检测器上分离维生素A、E,以多环芳烃柱为二维色谱柱,在二极管阵列检测器上分离维生素D2、D3和K1,建立在线固相萃取/二维液相色谱分析方法。对该方法进行方法验证,并与现行食品安全国家标准进行结果对比。维生素A、D、E、K1在标准曲线浓度范围内线性良好,维生素A、维生素D2、维生素D3、α-维生素E、β-维生素E、δ-维生素E、γ-维生素E和维生素K1检出限分别为4.0、1.0、1.0、40.0、40.0、40.0、40.0、4.0 μg/100g,定量限分别为10、2.5、2.5、100.0、100.0、100.0、100.0、10.0 μg/100g,加标回收率为91.23%~107.2%,相对标准偏差为0.67%~8.06%。该方法操作简单,重复性好,准确度高,能够满足婴幼儿配方奶粉中多种脂溶性维生素的同时检测。

关键词： 在线固相萃取; 二维液相色谱; 脂溶性维生素; 婴幼儿配方奶粉; 同时测定

本文引用格式

毛燕妮 , 许晴 , 李宏铨 , 聂懿 , 朱静璇 , 柳慧冰 , 康翠欣 . 在线固相萃取/二维液相色谱法同时测定婴幼儿配方奶粉中多种脂溶性维生素[J]. 食品与发酵工业, 2023 , 49(4) : 268 -273 . DOI: 10.13995/j.cnki.11-1802/ts.030970

Abstract

An analytical method to monitor fat-soluble vitamins A, D, E, and K1 in infant formula powder had been established which comprised online solid phase extraction (SPE) technique and two-dimensional liquid chromatography. The samples were saponified and purified by SPE column with PLRP-S polymer packing. vitamin A and vitamin E were separated by an ultraviolet detector using a pentafluorophenyl silica gel column as the one-dimensional chromatographic column. vitamin D2, D3, and vitamin K1 were segregated by a diode-array detector when the polycyclic aromatic hydrocarbons column was used as the two-dimensional column. Method validation was carried out and the feasibility of the method was compared with the national food safety standard method. Results showed that all the vitamins exhibited a good linear relationship in the range of the standard curve. The limit of detection (LODs) for vitamin A, vitamin D2, vitamin D3, α-vitamin E, β-vitamin E, δ-vitamin E, γ-vitamin E, and vitamin K1 were 4.0, 1.0, 1.0, 40.0, 40.0, 40.0, 40.0, 4.0 μg/100g, respectively. The limit of quantitation (LOQs) was 10.0 μg/100g for vitamin A and vitamin K1, 2.5 μg/100g for vitamin D2 and vitamin D3, 100.0 μg/100g for α-vitamin E, β-vitamin E, δ-vitamin E, and γ-vitamin E. The recoveries were in the range of 91.23%-107.2% and the relative standard deviation (RSD) ranged from 0.67% to 8.06%. The method is simple, has high sensitivity and good reproducibility, and can be employed perfectly to simultaneously analyze eight fat-soluble vitamins in the infant formula.

Key words： online solid phase extraction; two-dimensional liquid chromatography; fat-soluble vitamins; infant formula; simultaneous determination

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