Kong Yu, Yuan Jiaqiang, Wang Zilong, Hou Zhanwu, Yu Jiang, Jin Han, Xie Meihua, Chang Nan, Xu Weiyong, Zhao Yongxi, Tang Yuhai
The Key Laboratory of Biomedical Information Engineering of Ministry of Education, School of Life Science and Technology, Xi'an Jiaotong University, Xi'an, P.R. China.
J Sep Sci. 2014 Mar;37(6):717-24. doi: 10.1002/jssc.201300603.
A pH-mediated stacking method in capillary electrophoresis as an assay for low concentrations of melamine in milk products was established. Real samples were treated with acetone and sodium acetate and injected directly after centrifugation and filtration. Several experimental factors, such as buffer pH, buffer concentration, sample matrix, injection/sweeping ratio, sweeping time/voltages, separation voltages, as well as sample pretreatment, which affected stacking and separation, were investigated and optimized. Under the selected condition, a low LOD of 0.01 μmol/L (S/N = 5) and a wide range of linearity of 0.01∼1.0 μmol/L could be easily achieved with a good reproducibility (RSDs < 5.8% for both migration time and peak area) and an acceptable recovery of 94.0∼103.2% (for milk, infant formula, yogurt, and milk products). The proposed method was suitable for routine assay of melamine in real milk samples.
建立了一种用于毛细管电泳的pH介导堆积方法,作为测定乳制品中低浓度三聚氰胺的分析方法。实际样品用丙酮和醋酸钠处理,经离心和过滤后直接进样。研究并优化了几个影响堆积和分离的实验因素,如缓冲液pH值、缓冲液浓度、样品基质、进样/推扫比、推扫时间/电压、分离电压以及样品预处理。在选定条件下,可轻松实现0.01 μmol/L的低检测限(S/N = 5)和0.01∼1.0 μmol/L的宽线性范围,具有良好的重现性(迁移时间和峰面积的相对标准偏差均< 5.8%)和94.0∼103.2%的可接受回收率(针对牛奶、婴儿配方奶粉、酸奶和乳制品)。该方法适用于实际牛奶样品中三聚氰胺的常规检测。