食品科学 ›› 2010, Vol. 31 ›› Issue (6): 227-229.doi: 10.7506/spkx1002-6630-201006054

• 分析检测 • 上一篇    下一篇

高效阴离子交换色谱法测定生鲜乳中硫氰酸盐的含量

孟利   

  1. 黑龙江大学生命科学学院
  • 收稿日期:2009-04-23 修回日期:2009-09-27 出版日期:2010-03-15 发布日期:2010-12-29
  • 通讯作者: 孟利 E-mail:mengli198026@126.com
  • 基金资助:

    黑龙江大学博士启动基金项目

High Performance Ion Chromatographic Determination of Thiocyanate in Fresh Milk

MENG Li   

  1. College of Life Science, Heilongjiang University, Harbin 150080, China
  • Received:2009-04-23 Revised:2009-09-27 Online:2010-03-15 Published:2010-12-29
  • Contact: MENG Li E-mail:mengli198026@126.com

摘要:

建立高效阴离子交换色谱电导法分析生鲜乳中硫氰酸盐的方法。采用乙酸溶液沉淀生鲜乳中蛋白,过滤后用RP 柱去除样品中的脂类物质。净化后,直接将试样注入离子色谱仪分离,淋洗液OH-浓度为60mmol/L,外标法定量。稳定性实验中5 次进样1mg/L 硫氰酸根溶液的保留时间平均值为15.445min(RSD 为0.12%),峰面积平均值为0.1839μS·min(RSD 为0.26%)。方法回收率为96.0%~98.0%,RSD < 1.06%,检测限为0.2mg/kg,线性范围为0.5~6mg/L。

关键词: 生鲜乳, 硫氰酸盐, 阴离子交换色谱

Abstract:

A high performance ion chromatographic (HPIC) method was developed for determining thiocyanate in fresh milk. Samples were added with 3.0% acetic acid aqueous solution to precipitate protein and filtrated. The filtrate obtained was cleaned up using Dionex OnGuard RP cartridge for the removal of lipids prior to chromatographic separation. The elutant was adjusted to contain 60 mmol/L hydroxyl ions. The external standard method was used for thiocyanate quantification. Stability experiments gave an average retention time and an average peak area of 5 injection replicates of thiocyanate of 15.445 min and 0.1839 μS·min, with RSDs of 0.12% and 0.26%, respectively. Spike recoveries of thiocyanate in milk power and fresh milk at two levels ranged from 96.0% to 98.0%, with RSDs of less than 1.06%. The method exhibited a limit of detection of 0.2 mg/kg and a linear range of 0.5 to 6 mg/L.

Key words: fresh milk, thiocyanate, high performance ion chromatography (HPIC)

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