研究简报 Short communications

正相液相色谱法测定饲料添加剂天然维生素E中的生育酚和生育三烯酚的含量

  • 王石 ,
  • 王继彤 ,
  • 王燕妮 ,
  • 肖志明 ,
  • 贾铮 ,
  • 李阳 ,
  • 刘晓露 ,
  • 樊霞
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  • 1. 中国农业科学院农业质量标准与检测技术研究所, 北京 100081;
    2. 北京市饲料监察所, 北京 100107;
    3. 中国农业机械化科学研究院, 北京 100083
王石(1987-),男,北京人,助理研究员,硕士,从事饲料质量与安全检测技术研究。E-mail:wangshi01@caas.cn

收稿日期: 2019-05-24

  网络出版日期: 2019-12-13

基金资助

“十三五”国家重点研发计划项目课题(2016YFF0201802);国家标准制定项目(20100303-T-469);中央级公益性科研院所基本科研业务费专项(Y2019PT01)

Determination of Tocopherol and Tocotrienol Contents in Natural Vitamin E of Feed Additive by Normal Phase Liquid Chromatography

  • WANG Shi ,
  • WANG Jitong ,
  • WANG Yanni ,
  • XIAO Zhiming ,
  • JIA Zheng ,
  • LI Yang ,
  • LIU Xiaolu ,
  • FAN Xia
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  • 1. Institute of Quality Standards&Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China;
    2. Beijing Feed Testing Institute, Beijing 100107, China;
    3. Chinese Academy of Agricultural Mechanization Sciences, Beijing 100083, China

Received date: 2019-05-24

  Online published: 2019-12-13

摘要

天然维生素E因具有促进动物生长、提高肉品质等功能,已被逐步用于宠物及畜禽饲养,但行业中尚无规范该类饲料及饲料添加剂产品的标准及检测方法。本研究旨在建立采用正相液相色谱-紫外检测器(NPLC-UV)测定饲料添加剂中8种天然维生素E含量的分析方法。样品经甲醇浸润后,以乙酸乙酯/正己烷(3:97,V/V)为提取溶剂在室温下进行超声浸提。使用Kromasil 60-5 diol (4.6 mm×150 mm)色谱柱进行分离,正庚烷/四氢呋喃(100:4,V/V)等度洗脱,流速1.0 mL/min,柱温40℃,紫外检测波长为292 nm。结果表明:生育酚和生育三烯酚含量在0.2~50.0 μg/mL时线性关系良好(R2≥0.999 0),方法定量限为0.01%,加样平均回收率为81.3%~109.8%,相对标准偏差(RSD)小于7.9%。通过对实际样品测定,该方法操作简单,结果准确可靠,有助于规范天然维生素E饲料产品市场。

本文引用格式

王石 , 王继彤 , 王燕妮 , 肖志明 , 贾铮 , 李阳 , 刘晓露 , 樊霞 . 正相液相色谱法测定饲料添加剂天然维生素E中的生育酚和生育三烯酚的含量[J]. 动物营养学报, 2019 , 31(12) : 5823 -5833 . DOI: 10.3969/j.issn.1006-267x.2019.12.048

Abstract

The natural vitamin E has been gradually used in pets and livestock breeding because of it can promote the growth of animals and improve the meat quality. Nowadays, there are many kinds of feed additives containing natural vitamin E sold in the markets. However, the standard analytical methods have not yet been developed to monitor these products. In this work, an analytical method using normal phase liquid chromatography-ultraviolet and visible spectrophotometry (NPLC-UV) had been developed for the simultaneous determination of eight natural vitamin E contents. The samples were wetted with methanol and ultrasonic extracted using ethyl acetate/hexane (3:97, V/V). The target analytes were successfully separated on a Kromasil 60-5-diol column (4.6 mm×150 mm) with the mobile phase consisting of N-heptane/Tetrahydrofuran (100:4,V/V) at a flow rate of 1.0 mL/min. The column was thermostated at 40℃ and UV detection was performed at 292 nm. Good linearity was obtained in the ranges of 0.2 to 50 μg/mL, with linear coefficients (R2) higher than 0.999 0. The limit of detection (LOD) was 0.01%. Average recoveries from the fortification samples ranged between 81.3% and 109.8%, with relative standard deviations (RSD) lower than 7.9%. By analyzing the actual sample, the proposed method is reliable, sensitive and easy to perform, making it applicable for routine analysis to provide technical support for market regulation.

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