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以C18和MCX串联固相萃取柱作为净化手段,建立检测食品中违禁添加物乌洛托品含量高效液相色谱-串联质谱法(HPLC-MS/MS)的方法。在电喷雾正离子模式下,采用选择反应监测模式(SRM),用目标物的保留时间和质谱碎片丰度比来定性,外标法定量。结果表明,乌洛托品在0.5μg/L~1 000μg/L浓度范围线性良好,相关系数为0.998 9,方法的检出限为0.25μg/kg,定量限为2.5μg/kg,阴性样本添加水平为5μg/kg,10μg/kg和20μg/kg时,平均回收率为83.5%~105.1%,相对标准偏差(RSD)为0.9%~4.8%。方法具有准确、快速、简单以及灵敏度高的特点,能够适应大规模样品的快速分析要求。
A C18 and MCX tandem SPE column was used as a purification method to establish a HPLC-MS / MS method for the determination of hexachlorophenol, a banned additive in food. In electrospray positive mode, selective reaction monitoring (SRM) was used to characterize the target retention time and mass spectral fragment abundance ratio by external standard method. The results showed that urotropine had a good linearity in the range of 0.5μg / L to 1 000μg / L with a correlation coefficient of 0.998 9. The detection limit was 0.25μg / kg and the limit of quantification was 2.5μg / kg. Negative samples were added The average recoveries ranged from 83.5% to 105.1% with relative standard deviations (RSDs) from 0.9% to 4.8% at 5 μg / kg, 10 μg / kg and 20 μg / kg levels. The method is accurate, fast, simple and sensitive. It can adapt to the rapid analysis of large-scale samples.