反相高效液相色谱法测定饲料中尼卡巴嗪含量

Nicarbazin Determination in Feed by Reverse-phase High Performance Liquid Chromatography

用二甲基甲酰胺 (DMF)提取试样中的尼卡巴嗪 ,经碱性氧化铝层析柱过柱纯化、浓缩 ,并用洗脱液溶解、定容 ,用高效液相色谱仪C18反相柱 ,在波长 36 5nm、流速 1mL/min条件下对饲料中尼卡巴嗪含量进行测定。通过对氧化铝活性、层析柱高度、流动相等检测条件对比试验 ,建立的理想检测条件为 :10 5℃恒温干燥 2h处理高度 6cm的氧化铝柱 ,采用的流动相甲醇∶水为 80∶2 0。应用建立的测试方法 ,对饲料添加 10 0mg/kg尼卡巴嗪进行 30次重复试验。结果表明 ,尼卡巴嗪回收率在 91.9%～ 10 7.5 %之间 ,标准偏差 4 .0 %。研究还表明 ,饲料中其它常用的抗球虫药盐霉素、马杜霉素。

After extracting by dimethylformamide (DMF), homogenizing and concentrating by using alkaline alumina column, rinsing and fixing volume by lotion,then the nicarbazin in-feed was determined by reversed-phase high performance liquid chromatography with ultraviolet detection at 365 nm, 1 mL/min and C-18 sorbent. By a series of the experiments on comparing alumina activity, alumina column height, and methanol-water ratio, the optimal measurement condition was set as drying alumina with height 6 cm At 105,C for 2 hours under methanol-water ratio 80:20. The verify test was carried out through 30-replication by adding 100 mg/kg nicarbazin in feed., Nicarbazin recovery in feeds was ranged from 91.9% to 107.5% with relative standard deviation 4.0%. There was no interference from coccidiostat salinomycin, maduramasin and diclazuril when nicarbazin in feeds was measured with the method.