奶糖、巧克力三聚氰胺基质效应的研究和消除

Study and Elimination of Matrix Effect of Melamine in Milk Candy and Chocolate

试验选取8种奶糖和8种巧克力作为样品,用于探究液质联用在检测奶糖、巧克力中三聚氰胺基质效应的影响,并采用内标法消除基质效应。通过研究样品的取样量、溶剂的种类、溶剂的用量、三聚氰胺浓度和净化方式探讨基质效应,并通过软件SPSS 20进行显著性分析。结果表明,取样量、溶剂种类[除三氯乙酸和三氯乙酸-乙腈(4︰1,V/V)]、溶剂用量,以及不过SPE小柱和过SPE小柱之间对液质联用技术检测奶糖、巧克力都具有基质效应的影响,而三聚氰胺浓度和过不同SPE小柱及溶剂[三氯乙酸和三氯乙酸-乙腈(4︰1,V/V)]对三聚氰胺的基质效应无显著影响。研究表明,内标法能彻底消除基质效应的影响。

Eight kinds of milk sugar and chocolate were selected as samples to investigate the influence of liquid-mass combination on the matrix effect of melamine in milk sugar and chocolate,and the matrix effect was eliminated by internal standard method.The matrix effect was discussed by studying the sampling amount of samples,the type and amount of solvents,the concentration of melamine and the purification methods.The significance of the matrix effect was analyzed by SPSS 20.The results showed that the sample quantity,the types of solvents(except trichloroacetic acid and Vtrichloroacetic acid︰Vacetonitrile=4︰1),the amount of solvent and the influence of SPE column and superspee column on the matrix effect of liquid-mass combination technology were found.However,the matrix effect of melamine was not significantly affected by melamine concentration and over SPE column,solvent[trichloroacetic acid and trichloroacetic acidacetonitrile(4︰1,V/V)].The results showed that the internal standard method could eliminate the influence of matrix effect completely.