【摘要】 目的:建立奶粉中三聚氰胺的基质分散固相萃取-高效液相色谱快速分析方法。方法:试样加三氯乙酸与Tri-tonX-100振荡后离心,上清液经PSA-C18基质分散固相萃取净化,再经0.45μm滤膜过滤后高效液相色谱法测定。分离柱为Waters XBridge C18柱,流动相为乙腈-辛烷磺酸钠离子对试剂(10∶90,V/V),紫外检测器测定。结果:三聚氰胺在1.00μg/ml～100.0μg/ml范围内的线性良好(相关系数≥0.9991)。方法检出限为0.5 mg/kg,相对标准偏差为1.2%～2.9%,加标回收率为90.5%～99.1%。结论:基质分散固相萃取样品前处理方法简便、快速、有机试剂用量少且提取效率高,方法适用范围广,可用于多种乳制品中三聚氰胺含量的快速测定。更多还原

【Abstract】 Objective:To establish a method for rapid determination of melamine in milk powder by high performance liquid chromatography after matrix solid phase dispersion extraction.Methods: TritonX-100 and trichloroacetic acid were used for demulsification of samples,and after centrifugation,the supernatant was cleaned up by solid phase extraction using PSA and C18(4∶ 1,m/m) as dispersants,which was analyzed by Waters XBridge C18 column with volume ratio acetonitrile and sodium octane(pH=3) of 10∶ 90(V/V) and detected by ultraviolet detector.Results: The pretreatment method of sample and the chromatographic conditions of analysis were critically optimized and the results showed good linearities in the ranges from 1.00 μg/ml to 100.0 μg/ml with correlation coefficients(r) no less than 0.9991.The detection limit of the method was 0.5 mg/kg.The relative standard deviations(RSDs) were 1.2%~2.9%,and the recoveries were 90.5%~99.1%.Conclusion: The method has advantages of simplicity,high sensitivity and less pollutants,and could be widely used for analyzing the melamine in many kinds of milk products.更多还原