SPE-HPLC法测定鸡蛋中灭蝇胺—环丙氨嗪

Study on analytical method of cyromazine in eggs by SPE-HPLC

本试验研究建立了用NH2柱和97%乙腈水溶液做流动相洗脱测定鸡蛋中灭蝇胺-环丙氨嗪残留量的高效液相色谱法,鸡蛋均质后经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,环丙氨嗪在0.02～1.0 μg/ml浓度范围内呈线性相关,标准曲线的相关系数(r)为0.9998,在0.02,0.05,0.10 mg/kg添加浓度,回收率为84.5%～95.2%,变异系数为3.9%～6.8%.检测限为0.02 mg/kg,定量限低于0.05 mg/kg.

A high-performance liquid chromatography （HPLC） with NH2 column and 97% acetonitrile eluate to determine the cyromazine residues in eggs was described in this paper. The egg samples were extracted with acetonitrile containing 20% NH4OH,and cleaned upon by a Cls column solid-phase extraction （SPE）. The calibration curve for cyromazine was linear in a concentration range of 0.02 - 1.0μg/ml（ r = 0.9998） .The recoveries at levels of 0.02,0.05,0.10 mg/kg fortified samples ranged from 84.5% - 95.2%, with coefficient of variation of 3.9% - 6.8%. The limits of detection were 0.05 mg/kg and the limits of quantification less than 0.5 mg/kg.