QuEChERS-固相萃取-高效液相色谱-串联质谱法测定预制食品中丙烯酰胺的含量

Determination of acrylamide in prepared foods by QuEChERS-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  丙烯酰胺(Acrylamide,AA)  QuEChERS  固相萃取  预制食品  HPLC-MS/MS

英文关键词:acrylamide  QuEChERS  solid phase extraction  prepared food  high performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立一种测定预制食品中丙烯酰胺含量的QuEChERS-固相萃取-高效液相色谱-串联质谱法(solid phase extraction-high performance liquid chromatography-tandem mass spectrometry, SPE-HPLC-MS/MS)。方法 采用水提法, 结合QuEChERS以及CARB/SCX/PSA固相萃取小柱对预制食品中丙烯酰胺进行提取净化, 同时借助HPLC-MS/MS进行测定, 内标法定量。结果 在5~500 mg/L范围内, 线性相关系数大于0.997, 方法的定量限为10.0 μg/kg; 在3个添加水平(20、40、100 μg/kg)下的回收率在86.58%~108.84%, 相对标准偏差在1.60%~5.42%。结论 该方法简化了净化步骤, 缩短前处理时间, 节约成本, 提高效率, 且方法灵敏度高、准确度和精密度好, 可应用于预制食品中丙烯酰胺含量的批量测定。

英文摘要:

      Objective To establish a QuEChERS-solid phase extraction-high performance liquid chromatography- tandem mass spectrometry (SPE-HPLC-MS/MS) method for the determination of acrylamide in prepared food. Methods The acrylamide in prepared foods was extracted by water, and the extract was purified by combination with QuEChERS and CARB/SCX/PSA SPE columns. The analyte was quantified by HPLC-MS/MS with an internal standard. Results In the range of 5–500 mg/L, the correlation coefficient of linear regression was greater than 0.997, and the limit of quantitative the method was 10.0 μg/kg. The recovery rates were 86.58%–108.84% at 3 added levels (20, 40, 100 μg/kg) with standard deviations between 1.60%–5.42%. Conclusion This method can simplify the purification step, shorten the pretreatment time, save the cost and improve the efficiency with high sensitivity, good accuracy and precision, and can be applied to the batch determination of acrylamide content in prepared food.