鸡血清中三聚氰胺高效液相色谱检测方法的建立

Development of Analytical Method of Melamine Residues in Chicken Serum by HPLC

以鸡血清为研究对象,考察了不同洗涤液和洗脱液浓度对三聚氰胺提取效率的影响。建立了鸡血清中三聚氰胺残留的简便高效液相色谱法,该方法采用NH2柱作为色谱分析柱,95%乙腈水溶液为流动相,样品经阳离子交换固相萃取柱净化、富集后,在紫外检测器214 nm处用高效液相色谱仪测定,保留时间在14～15 min。三聚氰胺浓度在0.05～5.0μg/ml范围内,相关系数(r)为0.999 9;在空白鸡血清样品中添加0.1μg/ml、1.0μg/ml和5.0μg/ml浓度的回收率为78.05%～88.69%,相对标准偏差(RSD)为1.15%～8.33%;样品检测定量限为0.1μg/ml。

Chicken serum in this experiment was as the research object and the different washing liquid and the eluate concentration on the extraction efficiency of melamine were inspected. A simple high-performance liquid chromatography （HPLC） with NH2 column and 95% acetonitrile eluate to determine the melamine in chicken serum was described. Target analytes of samples were cleaned up and concentrated by HyperSep Retain-CX column solid-phase extraction （SPE）. A perfect separation for melamine was achieved and retention time was 14-15 min at 214 nm. The standard curve was linear in the concentration range from 0. 05 μg/ml to 5.0 μg/ml, with correlation coefficient of 0. 999 9. Recoveries of melamine at fortified levels of 0. 1 μg/ml, 1.0 μg/ml and 5.0 μg/ml ranged from 78.05% to 88.69% , with relative standard devia- tion of 1.15% -8.33%. The quantification limit was 0. 1 μg/ml.