高效液相色谱法测定水产品中三聚氰胺的含量

Determination of melamine in fishery products by high performance liquid chromatography

以罗非鱼、南美白对虾和鳗鲡为实验对象,建立了水产品中三聚氰胺的离子对反相液相色谱测定法。用三氯乙酸和乙酸锌溶液超声提取待测物,离心后上清液过MCX阳离子柱净化,氨化甲醇溶液洗脱,水浴氮气吹干,用甲醇水溶液定容过滤后供高效液相色谱(HPLC)分析,外标法定量。结果表明,三聚氰胺在0.5～100.0mg/L浓度范围内呈线性相关,相关系数R2=0.9999。加标水平在0.2～10.0mg/kg时,回收率为87.6%～94.3%,相对标准偏差为3.9%～7.1%,检出限为0.2mg/kg。

The analytical method of melamine in fishery products by ion-pair reversed-phase high performance liquid chromatograph was established.The samples were extracted with trichloroacetic acid and zinc acetate by the ultrasonic wave.Then the extracts were centrifugalized, purified with the cation exchange column.The analyte were eluted by ammonia methanol,reconstituted by methanol-water after dried under nitrogen.The samples were ready for determination using external stand quantitation.The calibration curves showed good linearity in the range of 0.5-100.0mg/kg for melamine.The correlation coefficient was 0.9999.The recoveries were 87.6%-94.3 % at spiking levels 0.2 - 10.0mg/kg. The relative standard deviations were 3.9%-7.1%. The detection limit of melamine was 0.2mg/kg.