QuEChERS-液相色谱-串联质谱法同时测定调味品中49种工业染料

Simultaneous determination of 49 kinds of industrial dyes in condiments by high performance liquid chromatography-tandem mass spectrometry based on QuEChERS

中文关键词:  调味品  工业染料  液相色谱-串联质谱法

英文关键词:condiments  industrial dyes  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立基于QuEChERS方法-液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时测定调味品中49种工业染料含量的分析方法。方法 样品用甲醇-乙腈(50:50, V:V)混合溶剂提取、结合QuEChERS样品前处理技术经C18材料净化处理后, 在正、负离子切换模式下以多反应监测(multiple reaction monitoring, MRM)模式检测。结果 在一定的浓度范围内, 49种染料呈良好线性关系, 相关系数大于0.97, 方法检出限(limits of detection, LODs)为0.10~11.54 μg/kg, 方法定量限(limits of quantitation, LOQs)为0.33~38.46 μg/kg, 当实际样品中添加水平在5~1000 μg/kg范围时, 平均回收率70.8%~114.7%, 重复性相对标准偏差(relative standard deviation, RSD, n=6)为0%~9.4%, 精密度相对标准偏差为0.4%~13.1%。结论 本方法操作简单、高效, 准确度与精密度高, 可同时测定多种工业色素, 适合于调味品中49种工业染料快速检测。

英文摘要:

      Objective To establish a method for simultaneous determination of 49 kinds of industrial dyes in condiments by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) based on QuEChERS. Methods The industrial dyes were extracted with methanol-acetonitrile (50:50, V:V), purified by QuEChERS method with C18 and then detected by HPLC-MS/MS, and identified by electrospray ionization in positive and negative mode under multiple reaction monitoring (MRM) mode. Results Within a certain concentration range, 49 dyes showed good linear relationships with correlation coefficients more than 0.97. The limits of detection (LODs) were in the range of 0.10-11.54 μg/kg and the limits of quantification (LOQs) were 0.33-38.46 μg/kg. The average recoveries of 49 dyes were from 70.8% to 114.7% at the spiked level range of 5-1000μg/kg, and the relative standard deviations of repeatability (RSDs, n=6) were 0%-9.4%, while the relative standard deviations of precision were 0.4%-13.1%. Conclusion The method is simple and efficient, with high accuracy and precision, and can simultaneously determine various industrial pigments, which is suitable for the rapid detection of 49 kinds of industrial dyes in condiments.