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作 者:陈旻实[1] 刘伟[1] 郑思远[1] 林柏玲[1]
机构地区:[1]福建出入境检验检疫局技术中心,福建省检验检疫技术研究重点实验室,福建福州350001
出 处:《福建分析测试》2012年第5期17-20,共4页Fujian Analysis & Testing
摘 要:建立了一种用液相色谱技术检测分析食品接触材料中三聚氰胺残留量的方法。样品采用0.1 mol/L盐酸作为提取溶液,70℃水浴超声提取。色谱分离采用NH2柱,流动相为V(乙腈):V(5mmol/L磷酸盐缓冲溶液,pH 6.5)=75:25,二极管阵列检测器检测。在优化条件下,三聚氰胺浓度在0.2-100 mg/L范围内与其峰面积线性关系良好,检出限(S/N=3)为0.02 mg/L。在100μg的添加水平下,三聚氰胺的回收率在80-99%之间,相对标准偏差(RSD)为2.80-4.32%。揭示了原料中三聚氰胺残留量与成型品的三聚氰胺迁移量的正相关关系。结果表明,该法简便、快速,可准确测定食品接触材料中三聚氰胺残留量。A novel High-performance liquid chromatographic method of determination of residue of melamine was developed. Samples were extracted with 0.1 mol/L hydrochloric acid at 70℃ by ultrasonic extractor. The separation was performed on NH2 column at 30℃ and the mobile phase of acetonitrile (5mmol/L) with PBS (pH=6.5) (75:25, V/V) of isocratic elution was pumped at a flow rate of 1.0 mL/min with DAD detector. Under optimized condition, the calibration curves was linear from 0.2 to 100mg/L with LOD (S/N=3)of 0.02 mg/L for MEL. The method provided recoveries of 80% - 99% in the spiked mass of 100μg, and the RSD was between 2.80% - 4.32%. A proportional relationship between residue of melamine in raw materials and migration of melamine in their molding articles was observed. The satisfied experimental results indicated that the proposed method can be directly used for the determination of residue of melamine in food contact materials and articles conveniently, rapidly and accurately.
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