气相色谱法测定食醋中邻苯二甲酸二丁酯及其不确定度评定

摘要

The content of dibutyl phthalate (DBP) in vinegar was determined by gas chromatography (GC),and the method was established and validated.The uncertainty evaluation was discussed simultaneously.The results showed that DBP had a good linear relationship in the range of 0.19-4.75 mg/L (R-2=0.999 9).The limit of detection was 0.01 mg/L,the relative standard deviation (RSD) of precision tests was 0.96％.The adding standard recovery rate was 90.14％-96.41％ and the RSD was 2.53％.The average content of DBP in the samples was (0.111 ±0.005) mg/L,which indicated the migration quantity of DBP in the tested samples did not exceed the relevant limit (0.3 mg/kg).The uncertainty of the method was mainly derived from the firing of standard curve,followed by the recovery rate of the sample pretreatment.%建立食醋中邻苯二甲酸二丁酯(DBP)的气相色谱测定方法,并进行方法学验证,同时对所建方法进行不确定度评定.结果表明,DBP在0.19～4.75 mg/L质量浓度范围内线性关系良好(R2=0.999 9),检出限为0.01 mg/L,精密度试验相对标准偏差(RSD)为0.96％,加标回收率在90.14％～96.41％之间,RSD为2.53％.样品中DBP平均检测结果为(0.111 ±0.005) mg/L,表明所测样品中DBP的迁移量均未超出相关规定的限量(0.3 mg/kg).该方法的不确定度主要来源于标准曲线的拟合,其次为前处理回收率.