Simultaneous determination of melamine and benzoquanamine in aqueous food simulants of food contact materials by high performance liquid chromatography
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摘要: 建立了食品接触材料水性模拟物中三聚氰胺和苯代三聚氰胺的高效液相色谱（HPLC）分析方法。样品根据拟装食品类型不同,经水、3%（w/v）乙酸水溶液、4%（v/v）乙酸水溶液、10%（v/v）乙醇水溶液、20%（v/v）乙醇水溶液或50%（v/v）乙醇水溶液6种不同水性模拟物提取,0.45μm滤膜过滤后直接由高效液相色谱分析。色谱分离采用强阳离子交换与反相C18混合填料分析柱（混合比例1∶4）,柱温35℃,流动相为乙腈-20mmol/L乙酸铵缓冲溶液（pH3.0）（40∶60,v/v）,流速为0.2mL/min,检测波长为240nm。结果表明:在优化的条件下,三聚氰胺和苯代三聚氰胺标准品在0.220mg/L浓度范围内,线性相关系数为0.99970.9999,方法定量限（S/N>10）为0.0150.033mg/dm2。在0.0250.70mg/dm2三个水平加标测试,平均回收率在80.0%103.3%之间,相对标准偏差（n=6）为0.5%4.0%。该方法前处理简单、分析速度快,可用于食品接触材料水性模拟物中三聚氰胺和苯代三聚氰胺的同时检测。Abstract: A new analytical method based on high performance liquid chromatography (HPLC) technique was developed for the simultaneous determination of melamine and benzoquanamine in aqueous food simulants of food contact materials. According to the type of the contacted food, the samples were extracted by water, 3% (w/v) acetic acid aqueous solution, 4% (v/v) acetic acid aqueous solution, 10% (v/v) ethanol aqueous solution, 20% (v/v) ethanol aqueous solution or 50% (v/v) ethanol aqueous solution. The extracted solutions were injected in HPLC column before the penetration through a 0.45 m microporous membrane. The separation was performed on a strong cation exchange and reversed phase C18mixed packing column (1∶4, by mixing ratio) at 35℃ and with acetonitrile-20mmol/L ammonium acetate buffer solution (pH=3.0) (40∶60, v/v) as the mobile phase at a flow rate of 0.2mL/min. The detection was performed at UV 240nm. Under the optimum conditions, the linear range was from 0.2 to 20.0mg/L with the linear correlation coefficients of 0.99970.9999. The limits of quantification (S/N≥10) were 0.0150.033mg/dm2. The mean recoveries were 80.0%103.3% in spiked level of 0.0250.70mg/dm2with the relative standard deviation (n=6) 0.5%4.0%. This method is simple, rapid and suitable for the simultaneous determination of melamine and benzoquanamine in aqueous food simulants of food contact materials.
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