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采用 HPLC-DAD 法分离和测定天然食品补充剂中的苦杏仁苷和非天然新苦杏仁苷。

Separation and determination of amygdalin and unnatural neoamygdalin in natural food supplements by HPLC-DAD.

机构信息

Department of Analytical Chemistry, Faculty of Natural Sciences, Comenius University in Bratislava , Bratislava , Slovak Republic.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2019 Oct;36(10):1445-1452. doi: 10.1080/19440049.2019.1650962. Epub 2019 Aug 9.

DOI:10.1080/19440049.2019.1650962
PMID:31397641
Abstract

This work is focused on separation and determination of amygdalin and its unnatural form neoamygdalin in natural food supplements. Reversed-phase high-performance liquid chromatography with a high-stability silica-based column with C functional group has been used for solving this problem. The effect of the mobile phase composition as well as the column temperature on the separation of the amygdalin epimers has been investigated. Isocratic elution using a mobile phase composed of 0.05% aqueous formic acid and acetonitrile achieved the required separation within 17 min. Under optimum chromatographic conditions, the developed method was validated and was applied for the determination of amygdalin epimers in natural food supplements containing apricot or peach kernels. A simple extraction method using methanol as an extractant supported by an ultrasonic bath was used with recovery in the range of 94.8% to 104.3%. The limit of detection and limit of quantification values for R-amygdalin were 0.13 mg/L and 0.40 mg/L, respectively. The developed method proved to be precise with the intra-day and inter-day relative standard deviation values less than 2.23%.

摘要

本工作专注于从天然食品补充剂中分离和测定苦杏仁苷及其非天然形式新苦杏仁苷。采用具有 C 官能团的高稳定性硅胶柱的反相高效液相色谱法来解决此问题。考察了流动相组成和柱温对苦杏仁苷差向异构体分离的影响。采用由 0.05%甲酸水溶液和乙腈组成的等度洗脱,在 17 分钟内实现了所需的分离。在最佳色谱条件下,对所建立的方法进行了验证,并应用于含有杏仁或桃仁的天然食品补充剂中苦杏仁苷差向异构体的测定。使用甲醇作为提取剂,超声浴辅助的简单提取方法,回收率在 94.8%至 104.3%之间。R-苦杏仁苷的检测限和定量限分别为 0.13 毫克/升和 0.40 毫克/升。所建立的方法具有较高的精密度,日内和日间相对标准偏差值均小于 2.23%。

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