试验建立了微流高效液相(μ-HPLC)测定奶粉中三聚氰胺的方法.该方法采用自组装微流液相装置,它主要由一个四通分流器、两根不同内径的空毛细管和毛细管在柱检测池组成,可灵活调整合适的背压.样品由超声离心提取,然后加入1%三氯乙酸沉淀蛋白净化.色谱条件:自制色谱柱(有效长度29 cm,总长37.5 cm,5μmODS;即十八烷基硅烷),流动相为乙腈-离子对缓冲液,检测波长230 nm.在添加浓度为0.1~1.2 mg/mL的范围内线性关系良好,相关系数R为0.996 0,平均回收率为93.25%.结果证明该方法简便、快捷、经济,可以作为检测三聚氰胺的有效手段.
To establish a analystical method assembling micro-high performance liquid chromatography(μ-HPLC) internal standard determination for melamine in milk powder.The micro installment was mainly composed of four valve splitting appliance,two different inside diameter empty capillary,capillary on-column detection cell,which could adjust the appropriate back pressure flexibly.The sample with 1% trichloroacetic acid precipitation protein purification.was extracted by the supersonic vibration and centrifugation extraction,The chromatographic column self-made(effective length 29 cm,total length 37.5 cm,5 μm ODS),the acetonitrile and ion pair buffer solution as mobile phase,detection wave length 230 nm.The goood linearity was abtained in the range of from 0.1 to 1.2 mg/mL,and the coefficient 0.996 0.The average recoveries of melamine are 93.25%.The method was simple,quickly,economy,satisfactory,and could meet the needs of determinnation of melamine in minlk powder.