UPLC-MS/MS法测定葡萄干中6种人工合成甜味剂

Determination of 6 Artificial Sweeteners in Raisin Using UPLC-MS/MS

该试验旨在建立超高效液相色谱-串联质谱(UPLC-MS/MS)测定葡萄干中安赛蜜、糖精钠、甜蜜素、阿斯巴甜、阿力甜和纽甜6种人工合成甜味剂的测定方法。样品经0.1%甲酸水提取,采用C_(18)色谱柱分离,以0.05%甲酸水和乙腈作为流动相进行梯度洗脱。采用电喷雾离子化,负离子扫描和多反应监测模式(MRM)检测,外标法定量。结果表明,6种甜味剂在1~200 ng/mL范围内线性关系良好,相关系数均大于0.99。6种甜味剂的方法检出限为1~2μg/kg,方法定量限为2.5~5μg/kg;在10,20和100μg/kg 3个添加水平下,平均回收率在81.5%~106.7%之间,相对标准偏差为1.7%~6.9%(n=6)。该方法简单、灵敏度高、分析时间短,适用于葡萄干中6种人工合成甜味剂的测定。

A method was established for determining 6 artificial sweeteners(acesulfame potassium,saccharin sodium,sodium cyclamate,aspartame,alitame and neotame)in raisin by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Samples were extracted with 0.1%formic water.A total of 6 artificial sweeteners were separated on a BEH C_(18)column with gradient elution using a mobile phase made up of 0.05%formic water and acetonitrile.The samples were detected under negative multiple reactions monitoring(MRM).The results were quantified by external standard method.The linearities of 6 artificial sweeteners were in the concentration range of 1-200 ng/mL,with the correlation coefficients higher than 0.99.The limits of detection(LOD)and the limits of quantitation(LOQ)of the method were 1-2μg/kg and 2.5-5μg/kg.When the spiked levels were 10,20 and 100μg/kg,the average spiked recovery rates were in the range of 81.5%-106.7%.The relative standard deviation(RSD,n=6)was 1.7%-6.9%.The method was simple,sensitive,rapid and suitable for the determination of 6 artificial sweeteners in raisin.