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。
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.
出处
《中国卫生检验杂志》
CAS
2011年第11期2595-2597,共3页
Chinese Journal of Health Laboratory Technology
基金
上海市卫生局青年科研资助项目(2008Y117)
