UPLC-MS/MS法测烘焙咖啡和速溶咖啡中丙烯酰胺

Determination of Arcylamide in Roast Coffee and Instant Coffee by UPLC-MS/MS

采用超高效液相色谱串联三重四极杆质谱法测定烘焙咖啡和速溶咖啡中丙烯酰胺。样品2.0 g经正己烷去脂和乙腈提取,MCX固相萃取柱净化,采用Waters BEH-C18色谱柱分离,以0.1%的甲酸水溶液和乙腈溶液为流动相进行梯度洗脱;质谱采用电喷雾离子源和多反应监测模式。结果显示,当丙烯酰胺的质量浓度为5.0~250.0μg/L时,线性关系良好,相关系数(r)>0.999,定量限为1.0μg/kg,空白样品在3个添加水平(1,5和10μg/kg)下的回收率为81.2%~89.3%,S_(RSD)为5.1%~6.3%(n=6)。该方法灵敏度及准确度良好,能满足咖啡中丙烯酰胺含量检测的要求。

This study investigated to determine of arcylamide in roast coffee and instant coffee by ultra-performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS).After 2.0 g samples were degreased with n-hexane,arcylamide was extracted with acetonitrile,and cleaned up on a MCX cartridge.The target analytes were separated on a Waters BEH-C18 column with gradient elution using a mobile phase made up of 0.1%formic acid solution and acetonitrile.Electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode were adopted in MS analysis.The results showed that concentration of arcylamides showed good linearity in the range of 5.0-250.0μg/L(r>0.999).The limits of detection were 1.0μg/kg.The spiked recovery rates were in the range of 81.2%-89.3%at 3 spiked levels(1,5 and 10μg/kg)for blank sample,and the relative standard deviation(S_(RSD))was 5.1%-6.3%(n=6).The method was sensitive and accurate.It could meet the requirements for the determination of arcylamide in coffee.