食品科学

• 成分分析 • 上一篇    下一篇

柱前衍生-反相高效液相色谱法检测富硒米曲霉中有机硒形态

李红卫1,王开萍1,吴 娱1,唐正江1,汤 飞1,刘国庆1,2,*   

  1. 1.合肥工业大学生物与食品工程学院,安徽 合肥 230009;2.安徽省皖江禽产业研究院,安徽 宣城 242000
  • 出版日期:2015-11-25 发布日期:2015-12-03
  • 通讯作者: 刘国庆
  • 基金资助:

    安徽省科技攻关项目(1401032006)

Determination of Organic Selenium Compounds in Selenium-Enriched Aspergillus oryzae by Pre-Column Derivatization-RP-HPLC Method

LI Hongwei1, WANG Kaiping1, WU Yu1, TANG Zhengjiang1, TANG Fei1, LIU Guoqing1,2,*   

  1. 1. School of Biotechnology and Food Engineering, Hefei University of Technology, Hefei 230009, China;
    2. Anhui Wan Jiang Poultry Industry Research Institute, Xuancheng 242000, China
  • Online:2015-11-25 Published:2015-12-03
  • Contact: LIU Guoqing

摘要:

建立高效液相色谱法测定富硒米曲霉中有机硒形态的分析方法。采用6 mol/L HCl溶液,50 ℃水解富硒米曲霉48 h,提取样品中的有机硒,4-氯-3,5-二硝基三氟甲苯柱前衍生,C18反相色谱柱(4.6 mm×250 mm,5 μm)分离,以乙腈-水(1∶1,V/V)和pH 6.8乙酸-乙酸钠缓冲液为流动相进行梯度洗脱,紫外检测波长:240 nm,测得富硒米曲霉中有机硒化合物主要是硒代胱氨酸,检出限(RSN=3)为0.680 mg/L,定量限(RSN=10)为2.244 mg/L,线性范围为5.0~100 mg/L,加标回收率为94.8%~105.8%,硒代胱氨酸的含量为1.25 mg/g。本方法简单、灵敏、重复性好,可适用于富硒米曲霉及相关产品中有机硒形态的检测分析。

关键词: 富硒米曲霉, 有机硒, 硒代氨基酸, 柱前衍生-反相高效液相色谱法

Abstract:

A reversed phase-high performance liquid chromatography (RP-HPLC) method for the determination of organic
selenium compounds in selenium-enriched Aspergillus oryzae was established. The extraction of organic selenium compounds
from samples was performed through hydrolysis with 6 mol/L HCl solution for 48 h at 50 ℃. After pre-column derivatization
with 4-chlorine-3,5-dinitrobenzotrifluoride (CNBF), the derivatives were separated on a C18 reversed-phase column through
gradient elution with acetonitrile-water and pH 6.8 acetic acid-sodium acetate buffer solution. UV detection was carried
out at 240 nm. The organic selenium compound in selenium-enriched A. oryzae was mainly selenocystine (SeCys2).
The limit of detection (LOD) (RSN = 3) was 0.680 mg/L and the limit of quantitation (LOQ) (RSN = 10) was 2.244 mg/L.
The linear range was 5.0–100 mg/L. The recoveries were in the range of 94.8%–105.8% and selenium-enriched A. oryzae
contained 1.25 mg/g selenocystine. This method is simple, sensitive and accurate, and could be used to determine organic
selenium compounds in selenium-enriched A. oryzae and related products.

Key words: selenium-enriched Aspergillus oryzae, organic selenium, selenoamino acids, pre-column derivatization-RP-HPLC

中图分类号: