超高效液相色谱-串联质谱法同时测定小麦粉中4种新型非法添加剂

Simultaneous determination of 4 kinds of new illegal additives in wheat flour by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  小麦粉  新型非法添加剂  超高效液相色谱-串联质谱法

英文关键词:wheat flour  new illegal additives  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定小麦粉中4种禁用成分。方法 样品经80%乙醇:乙腈(1:1, V:V)提取除杂后上机分析。采用Atlantis T3色谱柱、5 mmol乙酸铵+0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱, 采用多反应监测模式进行定性、定量分析。结果 4种化合物在各自线性范围内线性关系良好, 相关系数均≥0.9990。方法检出限为15 μg/kg (曲酸、苯甲羟肟酸)、30 μg/kg (噻二唑)、3 μg/kg (三聚硫氰酸钠盐); 回收率为80.2%~96.2%, 相对标准偏差为0.8%~4.4% (n=6)。结论 该方法前处理简单、灵敏度高、结果准确可靠, 适用于小麦粉中4种新型非法添加剂的定性定量检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 4 kinds of prohibited components in wheat flour by ultra performance liquid chromatography-tandem quadrupole mass spectrometry. Methods The samples were analyzed after extracted and purified by 80% ethanol and acetonitrile (1:1, V:V). The gradient elution was carried out on an Atlantis T3 column with 5 mmol ammonium acetate+0.1% formic acid aqueous solution and methanol as mobile phases. Qualitative and quantitative analyses were carried out using a multi-reaction monitoring mode. Results All compounds showed good linear relationships within their respective linear ranges, and the correlation coefficients were greater than or equal to 0.9990. The limits of detection were 15 μg/kg (kojic acid, benzoximic acid), 30 μg/kg (thiadiazole) and 3 μg/kg (sodium tripolythiocyanate); The recoveries were 80.2%-96.2%, and the relative standard deviations were 0.8%-4.4% (n=6). Conclusion This method has the advantages of simple pretreatment, high sensitivity, accurate and reliable results, and is suitable for the qualitative and quantitative determination of four new illegal additives in wheat flour.