QuEChERS结合超高效液相色谱-串联质谱法测定咖啡中丙烯酰胺

A rapid extraction, purification and determination method for acrylamide in coffee was established by using an improved QuEChERS method combined with ultra-high performance liquid chromatography - tandem mass spectrometry. The coffee samples were defatted with n-hexane, and acrylamide was extracted with a K_4[Fe(CN)_6] solution, then purified with diatomaceous earth and graphitized carbon black (GCB). It was separated by a CAPCELL CORE PC chromatographic column (100 mm×2.1 mm, 2.7 μm), with acetonitrile - 0.1% formic acid aqueous solution (containing 1 mmol/L NH4Ac) as the mobile phase and isocratic elution. The mass spectrometry adopted the positive ion multiple reaction monitoring (MRM) mode and was quantified by the internal standard method. The results showed that acrylamide had a good linear relationship in the concentration range of 0.01 - 10.0 μg/mL, with a correlation coefficient (r~2) of 0.9996, a detection limit of 0.05 mg/kg, a quantification limit of 0.15 mg/kg, a recovery rate range of 73.6% - 81.3%, and a relative standard deviation range of 4.7% - 6.7%.

采用改进的QuEChERS方法,结合超高效液相色谱-串联质谱法,建立了咖啡中丙烯酰胺的快速提取净化和测定方法。咖啡样品经正己烷除脂,以K_4[Fe(CN)_6]溶液提取丙烯酰胺后,用硅藻土和石墨化碳黑(GCB)净化,经CAPCELL CORE PC色谱柱(100mm×2.1mm,2.7μm)分离,以乙腈-0.1%甲酸水溶液(含1mmol/L NH4Ac)为流动相,等度洗脱;质谱采用正离子多反应监测(MRM)模式,内标法定量。结果表明,丙烯酰胺在0.01~10.0μg/mL浓度范围内线性关系良好,相关系数(r~2)为0.9996,检出限为0.05mg/kg,定量限为0.15mg/kg,回收率范围为73.6%~81.3%,相对标准偏差范围为4.7%~6.7%。