HPLC-MS/MS法测定水产品中11种水溶性合成着色剂

Simultaneous Determination of 11 Kinds of Water-Soluble Synthetic Colorants in Aquatic Products by Ultra-Performance Liquid Chromatography-tandem Mass Spectrometry

建立一种超高效液相色谱-串联质谱法同时检测水产品中11种水溶性合成着色剂的分析方法。样品经萃取缓冲溶液超声提取,乙醇沉降技术净化后,用Acquity UPLC CSH C18 (2.1μm×100 mm,1.7μm)色谱柱分离,在质谱多反应监测(multiple reaction monitoring,MRM)模式下检测,色谱峰面积外标法定量。11种着色剂在1~1 000ng/m L质量浓度范围内,线性关系良好,相关系数均在0.994以上,方法定量限在3~10μg/kg范围内。分别对多种样品进行5,20和50μg/kg这3个质量分数加标回收率试验,回收率范围为72.8%~114.6%,相对标准偏差为2.81%~6.82%(n=6)。该方法分析时间短、灵敏度高,适用于水产品中11种水溶性合成着色剂的检测。

Establish a method for the simultaneous determination of 11 kinds of water-soluble synthetic colorants in aquatic products by ultra-performance liquid chromatography-tandem mass spectrometry.The samples were extracted by ultrasonic extraction with extraction buffer solution,purified by ethanol precipitation technology separated by Acquity UPLC CSH C18(2.1 μm×100 mm,1.7 μm) chromatographic column,detected by mass spectrometry multi-reaction monitoring mode,and quantified by external standard method of chromatographic peak area.The 11 kinds of colorants showed good linear relationships in the range of 1-1 000 ng/mL with the correlation coefficient r≥0.994.The limits of quantification were 3-10 μg/kg,and the standard addition recoveries of 11 kinds of colorants were 72.8%-114.6% at the 3 kinds of spike levels of 5,20 and 50 μg/kg.The relative standard deviations were 2.81%-6.82%(n=6).This method had short analysis time and high sensitivity,and was suitable for the detection of 11 water-soluble synthetic colorants in aquatic products.