高效液相色谱法测定鸡蛋、牛奶和猪肉中环丙氨嗪及三聚氰胺的实验研究

Study on Analytical Method of Cyromazine and Melamine Residues in Egg,Milk and Pork with HPLC

本实验研究建立用NH2柱和97%乙腈水溶液做流动相洗脱测定鸡蛋、猪肉和牛奶中环丙氨嗪和三聚氰胺残留量的高效液相色谱法,样品均质后经NaOH和20%氨水乙腈溶液重复提取2次、浓缩、过C18固相萃取小柱净化等处理后上机检测,环丙氨嗪和三聚氰胺得到了很好的分离,各自的保留时间分别是8min和12min。标准曲线在0.01～1.0μg/ml浓度范围内呈线性相关,环丙氨嗪、三聚氰胺标准曲线的相关系数(r)分别为0.9999、0.9994。检测限为0.02mg/kg,定量限低于0.05mg/kg。

A high-performance liquid chromatography （HPLC） with NH2 column and 97% acetonitrile-water as mobile phase to determine the cyromazine and melamine residues in egg, milk and pork was described in this paper. Samples were treated with NaOH, extracted with acetonitrile containing 20% NH4OH, and cleaned up by using C18 column solid-phase extraction （SPEi. A perfect separation for cyromazine and melamine was achieved with their respective retention time 8 and 12 min. The calibration curves for cyromazine and melamine are linear in the concentration range of 0.01 to 1.0 μg/ml, with the correlation coefficients of 0.9999 and 0.9994, respectively. The detection limits of both the compounds is 0.02 mg/kg and the quantification limit is less than 0.05 mg/kg.