建立了柱前衍生高效液相色谱-串联质谱测定糕点中2,3-丁二酮分析方法.在弱酸性条件下,丁二酮与2,4-二硝基苯肼发生衍生反应后,采用HSS T3 色谱柱分离,在梯度洗脱条件下进行分析,外标法定量.丁二酮在0.81 ng/mL～52.0 ng/mL浓度范围内线性相关系数良好(r≥0.999),方法的定量限为4.5µg/kg,加标回收率为 87.0%～93.8%,相对标准偏差为2.7%～3.3%.该方法操作简便、灵敏度高,可应用于糕点样品中丁二酮含量的测定.
Determination of Butanedione in Pastry by Pre-column Derivatization High Performance Liquid Chromatography-mass
A method for the determination of butanedione(2,3-butanedione)in pastry by pre-column derivatization high performance liquid chromatography-mass.Butanedione from pastry can react with 2,4-dinitrophenyl hydrazine under weak acid condition.The target analyte was separated by HSS T3 column with gradient elution using 0.1%formic acide solution and acetonitrile,which was quantified by external standard method.The experimental results demonstrated that the target analyte has good linearity in the concentration range of 0.81 ng/mL～52.0 ng/mL with correlation coefficients(r)above 0.999.The limit of quantitation was 4.5 µg/kg,and the recoveries were in the range 87.0%～93.8%,with the relative standard deviations were 2.7%～3.3%.The method was simplicity,high sensitivity and suitable for the quantitative of butanedione in pastry products.
NETL
NSTL
万方数据
