Issue 9
May. 2023
Turn off MathJax
Article Contents
HUANG Yan, LIN Lingchao, JIANG Tingting, et al. Simultaneous Determination of Vitamins A, D and E in Children's Formula Milk Powder by Combining Online Solid Phase Extraction and Two-Dimensional Liquid Chromatography[J]. Science and Technology of Food Industry, 2023, 44(9): 317−323. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022060239
Citation: HUANG Yan, LIN Lingchao, JIANG Tingting, et al. Simultaneous Determination of Vitamins A, D and E in Children's Formula Milk Powder by Combining Online Solid Phase Extraction and Two-Dimensional Liquid Chromatography[J]. Science and Technology of Food Industry, 2023, 44(9): 317−323. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022060239

Simultaneous Determination of Vitamins A, D and E in Children's Formula Milk Powder by Combining Online Solid Phase Extraction and Two-Dimensional Liquid Chromatography

doi: 10.13386/j.issn1002-0306.2022060239
  • Received Date: 27 Jun 2022
  • Issue Publish Date: 01 May 2023
  • A method was developed for the simultaneous determination of fat-soluble vitamins A, D2, D3 and α-, β-, γ-, δ-vitamin E in children's formula milk powder by combining online solid phase extraction (SPE) and two-dimensional liquid chromatography. The saponified samples were directly injected into the constructed system and purified by using the polymeric-based PLRP-S column as the SPE column. Then the target analytes were eluted in back-flush mode from the SPE column by SPE pump and refocused on the head of the first-dimensional column by using online dilution. Vitamins A and four E homologues were separated on a NuovaSilTM PFP column (4.6 mm×150 mm, 3 μm) as the first-dimensional column using a mobile phase consisting of methanol and 0.1% formic acid in water by gradient elution, and vitamins D2 and D3 were separated on a ChromCore PAH column (4.6 mm×150 mm, 3 μm) as the second-dimensional column using a mobile phase consisting of methanol and acetonitrile (90:10, v/v). The results showed good linearity in the range of 5.0~500.0 ng/mL for vitamin A, 1.0~100.0 ng/mL for vitamin D and 50.0~5000.0 ng/mL for vitamin E, and the correlation coefficients were all better than 0.9999. The limits of quantification for vitamins A, D2, D3 and α-, β-, γ-, δ-vitamins E were 5.11, 1.22, 1.25, 83.82, 57.27, 56.61, 54.82 µg/100 g, respectively. The spiked recoveries were 91.20%~104.47%, and the relative standard deviations were 0.94%~3.34%. The results show that the method established in this paper has the advantages of simple pretreatment, high automation, high analytical efficiency, high accuracy and good reproducibility, and is suitable for the determination of vitamins A, D and E in children's formula milk powder.

     

  • loading
  • [1]
    贺媛媛, 贺陈龙, 李雅然, 等. 反复呼吸道感染患儿维生素A、D、E水平及免疫功能指标的相关性[J]. 贵州医科大学学报,2020,45(11):1347−1350. [HE Y Y, HE C L, LI Y R, et al. Correlation between the levels of vitamins A, D, E, and immune function indexes in children with recurrent respiratory infections[J]. Journal of Guizhou Medical University,2020,45(11):1347−1350.
    [2]
    李兵, 赵海燕, 屠瑞莹, 等. 食品中维生素D与25-羟基维生素D检测技术及含量分布研究进展[J]. 分析测试学报,2019,38(4):495−502. [LI B, ZHAO H Y, TU R Y, et al. Recent advances on determination techniques for vitamin D and 25-hydroxyvitamin D and their content distributions in foods[J]. Journal of Instrumental Analysis,2019,38(4):495−502. doi: 10.3969/j.issn.1004-4957.2019.04.020
    [3]
    纪建兵, 刘金祥, 王正军, 等. 血清维生素A和维生素E水平与小儿急性下呼吸道感染的相关性[J]. 解放军预防医学杂志,2019,37(2):136−138. [JI J B, LIU J X, WANG Z J, et al. Association between serum vitamin A and vitamin E levels and acute lower respiratory tract infection in children[J]. Journal of Preventive Medicine of Chinese People’s Liberation Army,2019,37(2):136−138. doi: 10.13704/j.cnki.jyyx.2019.02.051
    [4]
    王慧, 毕颖薇. 特发性矮身材儿童血清维生素A及维生素D的水平研究[J]. 中华临床医师杂志,2021,15(6):445−449. [WANG H, BI Y W. Study of serum vitamin A and vitamin D level in idiopathic short stature children[J]. Chinese Journal of Clinicians,2021,15(6):445−449.
    [5]
    FANALI C, D'ORAZIO G, FANALI S, et al. Advanced analytical techniques for fat-soluble vitamin analysis[J]. TrAC Trends in Analytical Chemistry,2017,87:82−97. doi: 10.1016/j.trac.2016.12.001
    [6]
    WOOLLARD D C, BENSCH A, INDYK H, et al. Determination of vitamin A and vitamin E esters in infant formulae and fortified milk powders by HPLC: Use of internal standardization[J]. Food Chemistry,2016,197(A):457−465.
    [7]
    魏帅, 吕宁, 梁成珠, 等. 婴幼儿配方乳粉中维生素A、E检测方法的比较研究[J]. 食品安全质量检测学报,2020,11(24):9083−9092. [WEI S, LÜ N, LIANG C Z, et al. Comparative study of analytical methods on vitamin A and vitamin E in infant formula[J]. Journal of Food Safety and Quality,2020,11(24):9083−9092. doi: 10.19812/j.cnki.jfsq11-5956/ts.2020.24.002
    [8]
    GILL B D, INDYK H E. Analysis of vitamin D2 and vitamin D3 in infant and adult nutritional formulas by liquid chromatography-tandem mass spectrometry: A multilaboratory testing study[J]. Journal of AOAC International,2018,101(1):256−263. doi: 10.5740/jaoacint.17-0149
    [9]
    中华人民共和国国家卫生和计划生育委员会, 国家食品药品监督管理总局. GB 5009.82-2016 食品安全国家标准食品中维生素A, D, E的测定[S]. 北京: 中国标准出版社, 2016

    National Health and Family Planning Commission of the People's Republic of China, China Food and Drug Administration. GB 5009.82-2016 National food safety standard-Detemination of vitamin A, D, E in food[S]. Beijing: Standards Press of China, 2016.
    [10]
    孙学文, 刘莹莹, 谢军, 等. 超高效液相色谱-串联质谱法同时测定特殊医学用途配方食品中5种脂溶性维生素[J]. 中国食品药品监管,2020(6):64−70. [SUN X W, LIU Y Y, XIE J, et al. Simultaneous determination of five fat-soluble vitamins in formula foods for special medical use by ultra performance liquid chromatography-tandem mass spectrometry[J]. China Food & Drug Administration Magazine,2020(6):64−70.
    [11]
    施鹏飞, 王晓薇, 王巧云, 等. 超高效液相色谱法测定乳及乳制品中维生素D的含量[J]. 食品安全质量检测学报,2020,11(7):2122−2129. [SHI P F, WANG X W, WANG Q Y, et al. Determination of vitamin D in milk and dairy products by ultraperformance liquid chromatography[J]. Journal of Food Safety and Quality,2020,11(7):2122−2129. doi: 10.19812/j.cnki.jfsq11-5956/ts.2020.07.017
    [12]
    吴新文, 马凯, 张世芹, 等. 高效液相色谱法同时测定婴幼儿配方乳粉中的维生素A、D3、E和β-胡萝卜素[J]. 食品安全导刊,2019(15):182−185. [WU X W, MA K, ZHANG S Q, et al. Simultaneous determination of vitamin A, D3, E and β-carotene in infant formula milk powder by high performance liquid chromatography[J]. China Food Safety Magazine,2019(15):182−185.
    [13]
    黄旭, 袁波, 刘家阳. 固相萃取-高效液相色谱法测定婴幼儿乳粉中维生素D3的含量[J]. 山东化工,2017,46(8):82−84. [HUANG X, YUAN B, LIU J Y. Determination of vitamin D3 in infant milk powder by SPE-HPLC[J]. Shandong Chemical Industry,2017,46(8):82−84. doi: 10.3969/j.issn.1008-021X.2017.08.029
    [14]
    程传民, 李云, 谷明, 等. 超高效液相色谱-串联质谱法测定饲料中维生素D3[J]. 中国饲料,2022(1):83−87. [CHENG C M, LI Y, GU M, et al. Determination of vitamin D3 in feed by ultra performance liquid chromatography-tandem mass spectrometry[J]. China Feed,2022(1):83−87.
    [15]
    张艳海, 其布勒哈斯, 金燕, 等. 在线二维液相色谱法同时测定婴幼儿和成人配方营养品中的维生素A、D3和E[J]. 色谱,2015,33(3):291−297. [ZHANG Y H, QIBULE H, JIN Y, et al. Simultaneous determination of vitamins A, D3 and E in infant formula and adult nutritions by online two-dimensional liquid chromatography[J]. Chinese Journal of Chromatography,2015,33(3):291−297. doi: 10.3724/SP.J.1123.2014.11009
    [16]
    赵玉富, 咸伟玥. 二维液相色谱法同时测定饲料中维生素A、维生素D3、维生素E[J]. 饲料博览,2019(4):51−54. [ZHAO Y F, XIAN W Y. Two-dimensional liquid chromatography method for the content determination of vitamin A, vitamin D3, vitamin E in feed[J]. Feed Review,2019(4):51−54. doi: 10.3969/j.issn.1001-0084.2019.04.013
    [17]
    HUANG B F, PAN X D, ZHANG J S, et al. Determination of vitamins D2 and D3 in edible fungus by reversed-phase two-dimensional liquid chromatography[J]. Journal of Food Quality,2020,2020:1−6.
    [18]
    林玉宙, 吴宏, 郭荣烁, 等. 二维液相色谱/双检测器法同时测定婴幼儿配方奶粉中维生素A、D3和E的含量[J]. 食品工业科技,2016,37(20):68−71, 77. [LIN Y Z, WU H, GUO R S, et al. Simultaneous determination of vitamin A, D3 and E in infant formula milk powder and rice flour by two dimensional liquid chromatography/double detector[J]. Science and Technology of Food Industry,2016,37(20):68−71, 77.
    [19]
    赵玉富, 刘晓玲, 咸伟玥, 等. 二维液相色谱同时测定婴幼儿配方乳粉中多种脂溶性维生素[J]. 中国乳品工业,2019,47(6):37−40. [ZHAO Y F, LIU X L, XIAN W Y, et al. Simultaneous determination of various fat-soluble vitamin in infant formula milk powder by two dimensional liquid chromatography[J]. China Dairy Industry,2019,47(6):37−40. doi: 10.3969/j.issn.1001-2230.2019.06.009
    [20]
    张丽媛, 戚绿叶, 周明昊, 等. 柱切换法液相色谱测定保健食品中的维生素A、D、E[J]. 食品科学,2021,13(5):46−48. [ZHANG L Y, QI L Y, ZHOU M H, et al. Determination of vitamin A, D and E in health food by column switching liquid chromatography[J]. Food Science,2021,13(5):46−48. doi: 10.7506/spkx1002-6630-20200924-292
    [21]
    陈建彪. 在线净化二维液相色谱快速检测食品中维生素A、D、E[J]. 食品安全质量检测学报,2019,10(6):1726−1733. [CHEN J B. Rapid detection of vitamin A, D and E in food by on-line purification two-dimensional high performance liquid chromatography[J]. Journal of Food Safety and Quality,2019,10(6):1726−1733. doi: 10.3969/j.issn.2095-0381.2019.06.054
    [22]
    FRANK J, CHIN X W D, SCHRADER C, et al. Do tocotrienols have potential as neuroprotective dietary factors?[J]. Ageing Research Reviews,2012,11:163−180. doi: 10.1016/j.arr.2011.06.006
    [23]
    PAN J L, ZHANG C J, ZHANG Z M, et al. Review of online coupling of sample preparation techniques with liquid chromatography[J]. Analytica Chimica Acta,2014,815:1−15. doi: 10.1016/j.aca.2014.01.017
    [24]
    DAVANKOV V, TSYURUPA M. Chapter 13-hypercrosslinked polystyrene as column packing material in HPLC[J]. Comprehensive Analytical Chemistry,2011,56:503−521. doi: 10.1016/S0166-526X(11)56013-1
    [25]
    DZHABIEVA S A, KURBATOVA S V. Sorbent effect on retention of benzotriazoles in RP HPLC[J]. Russian Journal of Physical Chemistry A,2015,89(10):1907−1913. doi: 10.1134/S0036024415100088
    [26]
    SYCHOW C S, ILYIN M M, DAVANKOV V A, et al. Elucidation of retention mechanisms on hypercrosslinked polystyrene used as column packing material for high-performance liquid chromatography[J]. Journal of Chromatography A,2004,1030(1−2):17−24. doi: 10.1016/j.chroma.2003.10.098
    [27]
    DAVANKOV V A, TSYURUPA M P. Structure and properties of porous hypercrosslinked polystyrene sorbents styrosorb[J]. Pure and Applied Chemistry,1989,61(11):1881−1888. doi: 10.1351/pac198961111881
    [28]
    SAIFUTDINOV B R, DAVANKOV V A, PETUKHOVA G A, et al. Thermodynamics of liquid-phase adsorption on hypercrosslinked polystyrene networks with ultimate degrees of crosslinking[J]. Doklady Physical Chemistry,2015,462(2):135−139. doi: 10.1134/S0012501615060056
    [29]
    WU D, NEDEV G K, LUCY C A. Retention mechanism of hypercrosslinked polystyrene silic hybrid phase in normal phase chromatography[J]. Journal of Chromatography A,2014,1370:50−55. doi: 10.1016/j.chroma.2014.10.018
    [30]
    WONG Y F, MAKAHLEH A, SAAD B, et al. UPLC method for the determination of vitamin E homologues and derivatives in vegetable oils, margarines and supplement capsules using pentafluorophenyl column[J]. Talanta,2014,130:299−306. doi: 10.1016/j.talanta.2014.07.021
    [31]
    中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会. GB/T 27404-2008 实验室质量控制规范 食品理化检测[S]. 北京: 中国标准出版社, 2008

    General Administration of Quality Supervision, Inspection and Quarantine of China, Standardization Administration of China. GB/T 27404-2008 Criterion on quality control of laboratories-Chemical testing of food[S]. Beijing: Standards Press of China, 2008.
  • 加载中

Catalog

    Figures(5)  / Tables(5)

    Article Metrics

    Article views(61) PDF downloads(0) Cited by()
    Proportional views
    Related

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return