【摘要】 建立了食品中三氯蔗糖的超高效液相色谱-电喷雾串联质谱(UPLC-MS/MS)测定方法。样品中的三氯蔗糖用水提取,简单除杂后根据样品基质选用HLB柱净化或用沉淀剂去除样品中的脂肪和蛋白质,用甲醇-水定容。经反相色谱柱分离后,采用多反应监测(MRM)负离子模式检测,定性离子对为m/z 395.07/358.90和397.07/360.90,其中m/z 395.07/358.90用于外标法定量。方法的定量下限为0.4 mg/kg;线性范围为0.2～20 mg/L;在0.4、4、10 mg/kg 3个加标水平下,白酒、调制乳和油炸花生3种样品中三氯蔗糖的回收率为85%～98%,相对标准偏差(n=6)为1.7%～5.0%。更多还原

【Abstract】 An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of sucralose in foodstuffs.The sample was extracted with water.Different purificatory methods like HLB cartridge purification or precipitators removing fat and protein were chosen according to different sample matrixs.The extract was separated with reversed-phase UPLC column using a binary eluent under isocratic conditions,and determined by tandem mass spectrometry under negative electrospray ionization mode with multiple reaction monitoring(MRM) mode.m/z 395.07/358.90 and m/z 397.07/360.90 were selected as two precursor-product ion pairs,in which m/z 395.07/358.90 was used for quantization.Under the optimal conditions,the calibration curve was linear over sucralose concentration in the range of 0.2-20 mg/L with quantitation limit of 0.4 mg/kg.The average recoveries of sucralose from Chinese spirit,modified milk and fried peanut kernels at three spiked levels of 0.4,4,10 mg/kg ranged from 85% to 98% with relative standard deviations(n=6) of 1.7%-5.0%.The method showed good simplicity,sensitivity and stability,and was suitable for the rapid determination of sucralose in foodstuffs.更多还原