高效液相色谱法检测饼干中的三聚氰胺

Determination of melamine in biscuits by high performance liquid chromatography

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 ODS100mm×4．6mm，5μm，流动相为乙腈：辛烷磺酸钠离子对试剂（pH3）=15：85（g／V），流速为1．0mL·min^-1，检测波长为210nm，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）．

A high performance liquid chromatography method was developed for the determination of melamine in biscuits. The biscuit samples were extracted by 1% trichloroaeetic acid solution and 2.2 lead acetate, and melamine was separated on a Hypersil ODS C18 column （ 100 mm×4.6 mm, 5μm ）. 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 0.2-10μg· 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.