高效液相色谱法检测饼干中的三聚氰胺

建立由高效液相色谱法检测饼干中三聚氰胺的方法。样品用1%三氯乙酸和2.2%乙酸铅超声提取,色谱柱为Hypersil ODS 100 mm×4.6 mm,5μm,流动相为乙腈∶辛烷磺酸钠离子对试剂(pH 3)=15∶85(V/V),流速为1.0 mL.min-1,检测波长为210 nm,柱温为40℃。三聚氰胺在0.2~10μg.mL-1范围内,有良好的线性关系。在空白样品中添加1、2和4μg.mL-1的标准工作液,平均回收率在80.5%~93.5%之间,相对标准偏差为7.7%(n=9)。

etermination of melamine in biscuits by high performance liquid chromatography

A high performance liquid chromatography method was developed for the determination of melamine in biscuits. The biscuit samples were extracted by 1% trichloroacetic acid solution and 2.2% lead acetate,and melamine was separated on a Hypersil ODS C_18 column (100 mm×4.6 mm,5 μm ). Acetonitrile and sodium 1-octanesulfonate solution(pH 3)(15∶85,V/V) were used as mobile phase at a flow rate of 1.0 mL·min～(-1). The detective wavelength was set as 210 nm by an ultraviolet detector.The temperature of column was 40 ℃. The linear ranges for melamine were 0.2-10 μg·mL～(-1). The average recovery rate of this method varied from 80.5% to 93.5% with the relative standard deviation of 7.7% (n=9) when blank sample was fortified standard working solution of 1,2 and 4 μg·mL～(-1).