食品科学 ›› 2022, Vol. 43 ›› Issue (4): 225-230.doi: 10.7506/spkx1002-6630-20201106-062

• 成分分析 • 上一篇    下一篇

柱切换法液相色谱测定保健食品中的VA、VD、VE

张丽媛,戚绿叶,周明昊   

  1. (浙江省食品药品检验研究院,浙江 杭州 310052)
  • 出版日期:2022-02-25 发布日期:2022-03-08
  • 基金资助:
    浙江省健康产品化妆品行业协会团体标准项目(T/ZHCA-YSP2019001)

Determination of Vitamins A, D and E in Health Foods Using Column-Switching Liquid Chromatography

ZHANG Liyuan, QI Lüye, ZHOU Minghao   

  1. (Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China)
  • Online:2022-02-25 Published:2022-03-08

摘要: 建立柱切换法液相色谱测定保健食品中VA、VD、VE含量的方法。参照GB 5009.82—2016《食品中维生素A、D、E的测定》样品前处理方法,以Agilent Poroshell 120 PFP(4.6 mm×100 mm,2.7 μm)为一维色谱柱,甲醇、水为流动相梯度洗脱,分离VA和VE的4 种异构体,以Agilent Zorbax Eclipse PAH(2.1 mm×100 mm,3.5 μm)为二维色谱柱,甲醇、乙腈为流动相梯度洗脱,分离VD2和VD3。以Agilent Poroshell 120 EC C18(4.6 mm×5 mm,4 μm)为捕获柱,捕获VD。根据VD在一维色谱柱上的出峰起止时间,确定柱切换时间。一维检测波长为325 nm和294 nm,二维检测波长为264 nm。以外标定量法测定VA、VD、VE的含量。结果表明,VA在2.50~50.0 μg/mL、VD在0.10~2.00 μg/mL、VE在5.00~100.0 μg/mL线性范围内线性良好,相关系数均大于0.999。回收率为86%~102%,相对标准偏差为1.5%~4.0%。表明该方法测定准确,适用于保健食品中VA、VD、VE的含量测定。

关键词: 二维液相色谱;VA;VD;VE;保健食品

Abstract: A method for the determination of vitamins A (VA), D (VD) and E (VE) in health foods by column-switching two-dimensional liquid chromatography was established. According to the sample pretreatment method specified in the national standard GB 5009.82-2016, VA and four isomers of VE were separated on an Agilent Poroshell 120 PFP column (4.6 mm × 100 mm, 2.7 μm) as one-dimensional chromatographic column using a mobile phase consisting of methanol and water by gradient elution, and VD2 and VD3 were separated on an Agilent Zorbax Eclipse PAH column (2.1 mm × 100 mm, 3.5 μm) by gradient elution using a mobile phase composed of methanol and acetonitrile. VD was captured on an Agilent Poroshell 120 EC C18 column (4.6 mm × 5 mm, 4 μm). According to the peak time of VD on the one-dimensional chromatographic column, the column switching time was determined. The one-dimensional detection wavelengths were 325 and 294 nm, and the two-dimensional detection wavelength was 264 nm. The analytes were quantified by external standard method. Results indicated that the calibration curves were linear in the range of 2.50-50.0 μg/mL for VA, and 0.10-2.00 μg/mL for VD, and 5.00-100.0 μg/mL for VE, and the correlation coefficients were all more than 0.999. The recoveries were 86%–102%, with relative standard deviations (RSD) of 1.5%–4.0%. The results suggest that the developed method is accurate and suitable for the determination of VA, VD and VE in health foods.

Key words: column-switching liquid chromatography; vitamin A; vitamin D; vitamin E; health foods

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