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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

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【作者】 邵庆均张金枝宣士荣朱聪英陈慧华沈琴芳许梓荣

【Author】 Shao Qingjun *1, Zhang Jinzhi , Xuan Shirong 2, Zhu Congying 2, Chen Huihua 2, Shen Qinfang 1, Xu Zirong 1 1(Key Laboratory for Feed and Animal Nutrition of the Ministry of Agriculture, Zhejiang University, Hangzhou 310029) 2(Zhejiang Feed Quality Supervision Institute, Hangzhou 310021)

【机构】 浙江大学农业部动物营养与饲料重点实验室浙江省饲料质量监督检察所浙江大学农业部动物营养与饲料重点实验室 杭州310029杭州310029杭州310020杭州310029

【摘要】 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、地克珠利对该检测无任何干扰

【Abstract】 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℃ 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.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2003年11期
  • 【分类号】O657.7
  • 【被引频次】12
  • 【下载频次】194
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