色谱

色谱

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基于QuEChERS前处理技术和弱阳离子交换色谱的牛奶和奶粉中三聚氰胺的快速检测方法

魏杰1, 郭志谋2*, 沈爱金2, 章飞芳1*, 梁鑫淼1,2   

  1. 1. 华东理工大学药学院, 上海 200237; 2. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2011-01-27 修回日期:2011-04-11 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 章飞芳,博士,主要研究方向为食品安全分析. 郭志谋,博士,主要研究方向为新型分离材料与分离技术
  • 基金资助:

    国家科技支撑计划项目(No. 2009BADB9B02)和上海市科委重点基础研究项目(No. 09JC1403900

Rapid analysis of melamine in milk and milk powder using QuEChERS approach coupled with weak cation exchange chromatography

WEI Jie1, GUO Zhimou2*, SHEN Aijin2, ZHANG Feifang1*, LIANG Xinmiao1,2   

  1. 1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China; 2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2011-01-27 Revised:2011-04-11 Online:2011-07-28 Published:2011-08-19

PDF

626

被引次数

18

摘要： 应用QuEChERS前处理技术,并结合弱阳离子交换色谱,建立了牛奶和奶粉中三聚氰胺的快速检测方法。样品使用医用酒精(乙醇含量75%)和一种新型脂肪吸附(LAS)材料超声振荡处理,在沉淀(吸附)蛋白质和脂肪的同时提取三聚氰胺,然后经8000 r/min离心,上清液过膜直接分析。色谱分析在弱阳离子交换色谱柱(WCX)上进行,采用2 mmol/L pH为3.8的磷酸二氢钾水溶液为流动相,在5 min内实现分离分析。结果表明,该方法在0.02～20 mg/L内线性相关系数大于0.9999。在1～50 mg/kg添加浓度范围内,牛奶的平均回收率为98.9%～105.2%,相对标准偏差(RSD)为0.9%～3.4%;奶粉的平均回收率为86.4%～102.9%, RSD为1.5%～6.7%。本方法的检出限为0.05 mg/kg(牛奶)和0.1 mg/kg(奶粉)。整个分析检测过程没有使用有毒有害有机溶剂,是一种绿色的分析方法。

关键词: QuEChERS方法, 快速分析, 奶粉, 牛奶, 弱阳离子交换色谱, 三聚氰胺

Abstract: A simple, rapid method for the determination of melamine in milk and milk powder was developed using QuEChERS approach coupled with weak cation exchange chromatography (WCX). The samples were extracted and cleaned-up by medicinal alcohol and lipid adsorbent (LAS) simultaneously, then centrifuged and filtered for high performance liquid chromatographic (HPLC) analysis. The separation was performed on a WCX column (150 mm×4.6 mm, 5 μm) with 2 mmol/L KH2PO4 (pH 3.8) as mobile phase. The flow rate was 1.5 mL/min and the detection wavelength was 208 nm. The injection volume was 20 μL and the column temperature was 30 ℃. Under the optimized conditions, good linearity was obtained in the range of 0.02~20 mg/L with a correlation coefficient (r2) of 0.9999. For samples spiked with melamine standard in the range of 1~50 mg/kg, the average recoveries of standard in the milk and milk powder were 98.9%~105.2% and 86.4%~102.9%, respectively. The relative standard deviations were 0.9%~3.4% and 1.5%~6.7%, respectively. The limits of detection (LOD, S/N≥3) were 0.05 mg/kg (milk) and 0.1 mg/kg (milk powder). The present method is green due to not use of the toxic organic solvents.

Key words: milk, milk powder, QuEChERS, rapid analysis, weak cation exchange chromatography (WCX), melamine