超高效液相色谱—串联质谱测定红烧老抽中六种合成色素的方法

Determination of six synthetic colorants in dark soy sauce by UPLC/MS/MS

建立了超高效液相色谱-串联质谱法（UPLC/MS/MS）同时测定红烧老抽中日落黄、柠檬黄、苋菜红、胭脂红、诱惑红、亮蓝等6种合成色素的方法。样品用水稀释后经过聚酰胺粉柱子净化,采用超高效液相色谱-串联质谱进行分析。采用0.02mol/L乙酸铵和甲醇作为流动相,梯度洗脱,流速为0.2mL/min,在7min内实现6种合成色素的良好分离。串联质谱条件是正离子模式电离,采用多反应监测模式（MRM）。6种色素在10-1000μg/L的范围内线性良好。6种色素的方法最低检出限是10μg/kg,加标回收率在80.0%～93.4%之间,相对标准偏差在2.4%～6.8%之间（n=6）。本方法分析快速、定性准确、检出限低,应用到基质复杂的老抽类液体复合调味料的检测中效果较佳。

A method of determination of six synthetic colorants including sunset yellow,lemon yellow,amaranth, carmine,allura red and brilliant blue in dark soy sauce by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry was developed. The sample diluted by water was cleaned up with solid phase extraction polyamide column,analyzed by UPLC/MS/MS. The mobile phase was 0.02mol/L ammonium acetate and methanol in gradient condition. The flow rate was 0.2mL/min. Using the best gradient condition,six synthetic colorants achieved the grate separation in 7min. The condition of tandem mass spectrometer was positive ionization, using the Multiple Reaction Monitoring mode. And all the six synthetic colorants had a good linearity in a concentration range of 10-1000ug/L. The detect limit of the method was 10ug/kg to all six synthetic colorants. The spiked recoveries of six colorants ranged from 80.0% to 93.4% ,with the RSDs of 2.4%N6.8%（n=6）. This method was rapid,showed good accuracy determination,and had a low limit of detection. It showed a satisfied effect of the testing in liquid multiple seasoning like dark soy sauce which had a complex matrix.