色谱 ›› 2020, Vol. 38 ›› Issue (7): 841-846.DOI: 10.3724/SP.J.1123.2019.11023

• 研究论文 • 上一篇    下一篇

高效液相色谱法分析植物油中9种抗氧化剂

赵慧男1, 张艳侠1, 薛霞1, 戴琨1, 郑文静1, 马骋1, 祝建华1, 刘艳明1,*(), 张峰2,*()   

  1. 1 山东省食品药品检验研究院, 山东 济南 250101
    2 中国检验检疫科学研究院, 北京 100176
  • 收稿日期:2019-11-26 出版日期:2020-07-08 发布日期:2020-12-10
  • 通讯作者: 刘艳明,张峰
  • 作者简介:张峰.Tel:53898008, E-mail:fengzhang@126.com
    刘艳明.Tel:81216719, E-mail:msymliu@163.com;
  • 基金资助:
    山东省重点研发计划(医用食品)(2019YYSP020);国家重点研发计划(2017YFC1601600);山东省自然科学基金(ZR2017MC069)

Analysis of nine antioxidants in vegetable oils by high performance liquid chromatography

ZHAO Huinan1, ZHANG Yanxia1, XUE Xia1, DAI Kun1, ZHENG Wenjing1, MA Cheng1, ZHU Jianhua1, LIU Yanming1,*(), ZHANG Feng2,*()   

  1. 1 Shandong Institute for Food and Drug Control, Ji'nan 250101, China
    2 Chinese Academy of Inspection and Quarantine, Beijing 100176, China
  • Received:2019-11-26 Online:2020-07-08 Published:2020-12-10
  • Contact: LIU Yanming,ZHANG Feng
  • Supported by:
    Shandong Key Point Research and Invention Program (Food for Special Medical Purpose, FSMP)(2019YYSP020);the National Key Research and Development Program of China(2017YFC1601600);Natural Science Foundation of Shandong Province(ZR2017MC069)

摘要:

建立了一种快速准确检测植物油中9种常用合成抗氧化剂的高效液相色谱方法。样品经甲醇溶剂提取,冷冻除脂,以甲醇-0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,采用XBridge C18色谱柱分离,二极管阵列检测器检测,外标法定量。实验对9种抗氧化剂标准储备液的稳定性及储存条件进行了系统性考察,在标准物质配制和前处理过程中引入抗坏血酸棕榈酸酯(AP),并优化AP使用量,提高目标物的稳定性和检测准确度。实验还考察了不同提取溶剂、净化方式等对抗氧化剂提取效率的影响。结果显示,9种目标化合物能够较好分离,在线性范围内具有良好的线性关系,相关系数(R2)≥0.999,定量限为0.6~3.0 mg/kg;加标回收率为85.3%~104.1%,相对标准偏差≤5.0%。该方法简便快捷,灵敏度高,回收率和重复性良好。

关键词: 高效液相色谱, 抗坏血酸棕榈酸酯, 抗氧化剂, 植物油, 稳定性

Abstract:

A method was developed for the determination of nine antioxidants in vegetable oils by high performance liquid chromatography (HPLC). The samples were extracted with methanol, and the fat in the samples was degreased by freezing. Separation of the targeted compounds was performed on an XBridge C18 column in gradient elution mode using methanol-0.1% (v/v) formic acid aqueous solution as the mobile phase. The analytes were detected using a diode-array detector by the external standard method. The stability and storage conditions for the nine antioxidants were systematically investigated. Ascorbyl palmitate (AP) was introduced into the preparation and pre-treatment of the targets. The concentration of AP was optimized to improve the stability and recovery of the targets. The effects of different extraction solvents and purification methods on the extraction efficiencies were discussed. The results showed that the nine antioxidants could be separated well under the optimized conditions. Good linear relationships in the linear range were obtained, and the correlation coefficients (R2) were greater than 0.999. The average recoveries of the nine antioxidants ranged from 85.3% to 104.1%, with RSDs of the method ≤5.0%. The limits of quantitation (LOQs) for the nine synthetic antioxidants were in the range of 0.6-3.0 mg/kg. The method is simple, rapid, sensitive, and it shows good recovery and reproducibility.

Key words: high performance liquid chromatography (HPLC), ascorbyl palmitate (AP), antioxidants, vegetable oils, stability