摘要
建立了亲水作用色谱-串联质谱(HILIC-MS/MS)法同时测定食品接触材料中三聚氰胺(MEL)、三聚氰酸一酰胺(ADE)和三聚氰酸(CYA)的方法。食品接触材料分别采用水、4%乙酸、10%乙醇和橄榄油在70℃烘箱浸泡4h。水基浸泡液过0.45μm微孔薄膜后进入色谱柱,橄榄油提取物以凝胶色谱法净化后进入色谱柱。在优化条件下,亲水作用色谱柱分离,电喷雾串联四极杆质谱检测器检测,分别在正、负离子模式下测定。MEL、ADE和CYA分别在5～100、2～200、2～200μg/L范围内线性关系良好(R>0.999)。检出限分别为4.0、8.0、8.0μg/L。在5.0μg/L的添加水平下,MEL、ADE、CYA的平均回收率在98.9%～106.3%之间,相对标准偏差在2.49%～5.44%之间。结果表明,该法可简便、快速、准确地同时测定食品接触材料中三聚氰胺及其衍生物的迁移量。
A HILIC-MS/MS method was developed to determine melamine （MEL）,ammelide （ cyanuric acid （CYA） in food contact materials. Samples were extracted with H2 O,4% acetic ethanol separately,then kept at 70 ℃ for 4 h,and filtered with 0.45μm microporous membr ADE） and acid, 10% ane before injected into the system. The olive oil extration solution was cleaned up by gel permeation chromatography （GPC）. Under the optimized conditions, MEL, ADE and CYA were separated,identified and quantitated on HILIC column by gradient mobile phase under the positive/negative electrospray ionization and multiple reaction monitor （MRM） mode. Linear responses were obtained with the concentration of analytes ranging from 5- 100 μg/L, 2 - 200 μg/L and 2 - 200μg/L for melamine, ammelide and cyanuric, respectively. The limits of detection were 4.0,8.0 and 8.0μg/L. The recoveries for the spiked samples ranged from 98. 9% -106. 3% with relative standard deviations of 2. 49% 5.44%. The method is simple, rapid, accurate, and is suitable for the determination of melamine and cyacuric acid in food contact products.
出处
《分析科学学报》
CAS
CSCD
北大核心
2012年第5期647-651,共5页
Journal of Analytical Science
基金
福建省科技计划重点项目(No.2009Y0001)
国家质量监督检验检疫总局2011年度科技计划
福建出入境检验检疫局科技计划(No.FK2010-22)
