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试验建立了应用高效液相色谱法检测渔用配合饲料及原料中三聚氰胺含量的方法。样品经三氯乙酸-乙酸铅-盐酸提取,MCX固相萃取净化后,应用MGC18色谱柱进行分离,柱温为30℃,流动相为庚烷磺酸钠-柠檬酸-乙腈,流速1ml/min,紫外检测器240nm检测。外标法定量,方法线性范围为0.2～10μg/ml,线性方程为y=86621x+718.98,相关系数R=1,检测限为2mg/kg。不同样品的加标回收率为84.6%～99.2%,相对标准偏差为1.8%～5.2%。
The experiment established a method of using high performance liquid chromatography to detect the content of melamine in the fishery compound feed and raw materials. The sample was extracted with trichloroacetic acid-lead acetate-hydrochloric acid, purified by MCX solid-phase extraction and separated on a MGC18 column with a column temperature of 30 ℃ and a mobile phase of sodium heptane sulfonate-citric acid-acetonitrile at a flow rate of 1 ml / min , UV detector 240nm detection. The linear range was 0.2 ~ 10μg / ml, the linear equation was y = 86621x + 718.98, the correlation coefficient was R = 1 and the limit of detection was 2mg / kg. The spiked recoveries of different samples ranged from 84.6% to 99.2% with relative standard deviations of 1.8% -5.2%.