在线固相萃取—二维液相色谱法快速测定婴幼儿谷类辅食中维生素A、D3、E含量及其不确定度评定
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1湖南英氏营养食品有限公司,湖南 长沙 410300;2国家农副产品质量检验检测中心(湖南)婴幼儿辅食联合研发实验室,湖南 长沙 410300;3湖南省产商品质量检验研究院,湖南 长沙 410007

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戴志勇(1978—),男,湖南英氏营养食品有限公司高级工程师。E-mail: daizhiyong@engnice.com

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Rapid determination and uncertainty evaluation of vitamins A, D3, and E content in cereal-based complementary foods for infants and young children by online solid phase extraction-two-dimensional liquid chromatography
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1Hunan Enoulite Nutritional Food Co., Ltd., Changsha, Hunan 410300, China;2Infant Complementary Food Joint R&D Lab of National Quality Inspection Center for Agricultural and Sideline Products (Hunan), Changsha, Hunan 410300, China;3Hunan Provincial Institute of Product and Goods Quality Inspection, Changsha, Hunan 410007, China

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    摘要:

    目的 建立一种基于在线固相萃取—二维液相色谱技术,实现同时快速测定婴幼儿谷类辅食中维生素A、D3、E含量。方法 样品皂化液经在线固相萃取净化后,维生素A、E通过一维色谱完成分离测定,维生素D3经一维初步分离转移至二维色谱完成分离测定,均采用外标法定量。结果 维生素A、D3、E在相应的浓度范围内线性关系良好,相关系数R2均大于0.999;定量限分别为1.62,0.308,13.9 μg/100 g;加标回收率为92.4%~109.2%,相对标准偏差为0.36%~3.08%。此外,维生素A、D3、E的扩展不确定度(k=2)分别为7.04%,17.0%,5.30%。结论 该方法提升了前处理的自动化程度,简便高效、准确可靠,可满足婴幼儿谷类辅食中脂溶性维生素的批量检测需要。

    Abstract:

    Objective To establish a rapid determination method for vitamin A, D3, and E content in cereal-based complementary foods for infants and young children by online solid phase extraction-two-dimensional liquid chromatography simultaneously.Methods Sample saponification solution is purified by online solid-phase extraction. Then, vitamin A and E are separated and detected by the first-dimension chromatography, while vitamin D3 is preliminarily separated in the first dimension and then transferred to the second-dimension chromatography for further separation and detection, with all quantification achieved by the external standard method.Results Vitamin A, D3, and E exhibit a good linearity in the concentration ranges, with correlation coefficients (R2) being more than 0.999. The limits of quantification (LOQ) are 1.62, 0.308, and 13.9 μg/100 g for vitamins A, D3, and E, respectively. The spike recoveries range from 92.4% to 109.2%, with relative standard deviations (RSD) between 0.36% and 3.08%. Additionally, the expanded uncertainties (k=2) for vitamin A, D3, and E are 7.04%, 17.0%, and 5.30%, respectively.Conclusion With high simplicity, efficiency, accuracy, and reliability, this method enhances the automation degree in sample pretreatment, meeting the needs of batch detection of fat-soluble vitamins in cereal-based complementary foods for infants and young children.

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龙强,赵涛,肖媚,等.在线固相萃取—二维液相色谱法快速测定婴幼儿谷类辅食中维生素A、D3、E含量及其不确定度评定[J].食品与机械,2026,42(5):68-76.
LONG Qiang, ZHAO Tao, XIAO Mei, et al. Rapid determination and uncertainty evaluation of vitamins A, D3, and E content in cereal-based complementary foods for infants and young children by online solid phase extraction-two-dimensional liquid chromatography[J]. Food & Machinery,2026,42(5):68-76.

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  • 收稿日期:2025-07-04
  • 最后修改日期:2025-11-24
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  • 在线发布日期: 2026-06-17
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