食品科学

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高效液相色谱法测定鸡蛋中5-乙烯基-1,3-噁唑烷-2-硫酮残留量

朱丽萍,王建萍,丁雪梅,曾秋凤,白世平,玄 玥,宿卓薇,张克英*   

  1. 四川农业大学动物营养研究所,动物抗病营养教育部重点实验室,四川 成都 611130
  • 出版日期:2016-09-25 发布日期:2016-09-26
  • 通讯作者: 张克英
  • 基金资助:

    “十二五”国家科技支撑计划项目(2014BAD13B04);四川省科技厅科技支撑计划项目(2014NZ0043;2014NZ0002)

Analysis of 5-Vinyl-1,3-oxazolidine-2-thione Residue in Eggs by HPLC

ZHU Liping, WANG Jianping, DING Xuemei, ZENG Qiufeng, BAI Shiping, XUAN Yue, SU Zhuowei, ZHANG Keying*   

  1. Key Laboratory for Animal Disease-Resistance Nutrition of China, Ministry of Education, Institute of Animal Nutrition,
    Sichuan Agricultural University, Chengdu 611130, China
  • Online:2016-09-25 Published:2016-09-26
  • Contact: ZHANG Keying

摘要:

建立一种用于测定鸡蛋粉中5-乙烯基-1,3-噁唑烷-2-硫酮(5-vinyl-1,3-oxazolidine-2-thione,5-VOT)残留量的高效液相色谱法,并探讨5-VOT在鸡蛋中的残留消除情况。选用450 只30 周龄的罗曼粉壳蛋鸡,随机分为3 组,分别饲喂含0%(对照组,处理1)、17.64%(处理2)、29.4%(处理3)菜粕的饲粮,饲喂12 周后各组均换饲对照组的饲粮4 周,实验期共16 周。实验采用乙腈提取鸡蛋粉中5-VOT,样品经超声、离心、旋转蒸干处理,用pH 7.0的磷酸钠缓冲溶液复溶,下层溶液离心后经0.45 μm无机滤膜过滤上机。结果表明,方法平均加标回收率在81.28%~103.28%之间,平均回收率、重复性及精密度的相对标准偏差分别为0.75%~5.17%、2.19%、0.82%,可满足鸡蛋中5-VOT残留量的测定;鸡蛋中5-VOT残留量随着蛋鸡饲粮中菜粕含量以及蛋鸡饲喂菜粕饲粮时间的延长而增加,处理组3菜粨饲喂12 周后5-VOT残留量高达1 837.45 ng/g;换饲对照组饲粮4 周后,鸡蛋中未检出5-VOT。

关键词: 高效液相色谱法, 鸡蛋, 5-乙烯基-1,3-噁唑烷-2-硫酮

Abstract:

The study was conducted to establish an analytical method for measuring 5-vinyl-1,3-oxazolidine-2-thione
(5-VOT) residue in eggs and to apply it on eggs from laying hens fed different levels of rapeseed meal (RSM). A total of 450
30-week-old Lohmann pink-shelled hens were randomly assigned to 3 dietary treatments, including 0%, 17.64% and 29.4%
RSM supplementation for 16 weeks (which was withdrawn during the last 4 weeks). 5-VOT was extracted with acetonitrile,
and then evaporated to dryness with a rotating evaporator under vacuum at 35 ℃. The 5-VOT was re-dissolved in 2 mL of
phosphate buffer (pH 7.0) and purified with 2 mL of n-hexane. Thereafter, the aqueous solution was transferred to a 2 mL
tube and centrifuged for 5 min at 12 000 r/min. The aqueous phase was passed through a 0.45 μm filter for HPLC analysis.
The average recovery rates of 5-VOT ranged from 81.28% to 103.28% with relative standard deviations (RSDs) between
0.75% and 5.17%. The RSDs of repeatability and precision were 2.19% and 0.82%, respectively. The further investigation
showed that 5-VOT concentrations in eggs linearly increased with the increase in either the level of dietary RSM or feeding
time. After 4 weeks of RSM withdrawal, 5-VOT residue was not detected in eggs.

Key words: high performance liquid chromatography, egg, 5-vinyl-1,3-oxazolidine-2-thione

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