高效液相色谱-串联质谱法同时测定糖果中24种添加剂含量

Simultaneous Determination of 24 Additives in Candy by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了糖果中24种添加剂的高效液相色谱-串联质谱检测方法。样品经50%乙腈超声提取后,取上清液过聚四氟乙烯滤膜,滤液直接上机分析,在电喷雾电离模式下采用多反应监测模式进行测定。结果显示,24种添加剂在0.01~1.0μg/mL线性良好,线性相关系数大于0.995,方法检出限为2~124μg/kg,空白样品加标平均回收率为81.29%~106.33%,相对标准偏差为0.92%~9.11%。将该方法应用于市售糖果的检测,发现部分样品中胭脂红、甜蜜素、羟苯甲酯超出我国限量要求。该方法简单、快速,可用于糖果中添加剂的快速筛查。

A liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for determination of 24 additives in candies was developed.Samples were extracted by 50% acetonitrile by ultrasound,and then filtered by polytetrafluoroethylene filter membrane,the filtrate was directly for analysis.Mass spectral data were acquired in electro spray ion(ESI)mode using multiple reaction monitoring(MRM)scan function.Results showed that an excellent linear relationship in the range of 0.01~1.0μg/mL was observed for 24 additives with a correlation coefficient larger than 0.995.The limits of detection were 2~124μg/kg,the recoveries from spiked blank samples ranged from 81.29% to 106.33% with relative standard deviation between 0.92% and 9.11%.Carmine,sodium cyclamate,methyl 4-hydroxybenzoate levels exceed the national maximum limit were detected in some real samples by this method.The method is simple and rapid,and can be used for quick screening of additives in candies.