在线净化-二维液相色谱法测定特殊医学用途配方食品中维生素A、D、E
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作者单位:

江苏省疾病预防控制中心,江苏 南京 210009

作者简介:

韦娟 女 主管技师 研究方向为食品安全工作 E-mail:1326673879@qq.com

通讯作者:

吉文亮 男 主任技师 研究方向为理化检验 E-mail:641827872@qq.com

中图分类号:

R155

基金项目:

江苏省科学技术厅社会发展面上项目(BE2023772)


Determination of Vitamin A, Vitamin D and Vitamin E in formulas for special medical purposes by online purification-two-dimensional liquid chromatography
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Jiangsu Provincial Center for Disease Control and Prevention, JiangsuNanjing210009, China

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    摘要:

    目的 利用双阀三泵中心切割二维液相色谱技术,建立了一种在线净化-二维液相色谱法,用于测定特殊医学用途配方食品中维生素A、D、E(VA、VD、VE)的含量。方法 样品在经过皂化处理后,进入二维液相色谱系统。采用耐强碱溶液的PLRP-S小柱作为在线固相萃取柱,用于净化样品皂化液。随后,SPE泵反向洗脱目标物到一维色谱系统。选择全氟苯基柱作为分离VA和4种VE的一维色谱柱。同时,以C18小柱作为VD的捕获柱,多环芳烃柱作为分离VD2和VD3的二维色谱柱。结果 VA、VD、VE在不同浓度范围内呈现出良好的线性关系,其线性范围分别为0.010 0~1.000、0.001 00~0.100、0.200~20.0 μg/mL,相关系数均高达0.999 9。检出限分别为4.8、0.8和48 μg/100 g,定量限分别为12、2和120 μg/100 g。低、中、高3个不同加标水平下,VA、VD、VE的平均回收率表现良好,范围为85.9%~114.0%,相对标准偏差范围为0.6%~9.2%。结论 该方法操作简便,具有高灵敏度和良好的准确度,适用于特殊医学用途配方食品中VA、VD、VE的常规快速检测。

    Abstract:

    Objective To determine vitamin A (VA), vitamin D (VD) and vitamin E (VE) in formulas for special medical purposes, the online purification-two-dimensional liquid chromatography technique with dual-valve triple-pump center-cutting was established.Methods After the saponification, the samples were introduced into a two-dimensional liquid chromatography system. A PLRP-S column, which was resistant to strong alkaline solutions, was used as an online solid phase extraction column for the clean-up of the sample solution. Subsequently, SPE pumps were reversed to elute the target to the one-dimensional chromatographic system. A perfluorophenyl column was used as the 1D column for the separation of VA and the four VE species. Meanwhile, a C18 column was used as a capture column for VD and a polycyclic aromatic hydrocarbon column was used as a two-dimensional chromatographic column for the separation of VD2 and VD3.Results VA, VD and VE exhibited good linearity within different concentration ranges. The linear ranges were 0.010 0-1.000, 0.001 00-0.100, 0.200-20.0 μg/mL, and the correlation coefficients were all as high as 0.999 9. The limits of detection (LODs) were 4.8, 0.8 and 48 μg/100 g, and the limits of quantification (LOQs) were 12, 2 and 120 μg/100 g. The average recoveries of VA, VD and VE were good with the ranges of 85.9%-114.0%, and the relative standard deviations (RSDs) ranged from 0.6% to 9.2% for the different spiked levels of low, medium and high.Conclusion The method is easy to operate, with high sensitivity and good accuracy, and it is suitable for the routine rapid determination of VA,VD and VE in formulas for special medical purposes.

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韦娟,张昊,王溪,霍宗利,吉文亮.在线净化-二维液相色谱法测定特殊医学用途配方食品中维生素A、D、E[J].中国食品卫生杂志,2024,36(9):1017-1023.

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  • 收稿日期:2024-03-28
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  • 在线发布日期: 2025-01-01
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