超高压液相色谱-串联质谱法测定速溶咖啡和曲奇饼干中丙烯酰胺的含量

Determination of Acrylamide in Instant Coffee and Cookies by UHPLC-MS/MS

建立了超高压液相色谱-串联质谱法(UHPLC-MS/MS)测定速溶咖啡和曲奇饼干中丙烯酰胺含量的方法。分别称取速溶咖啡或曲奇饼干样品2.0 g,用乙腈提取2次(10 mL×2),正己烷除脂2次(10 mL×2),取10 mL乙腈相于40℃减压浓缩至近干,加水1 mL溶解,经0.45μm水系滤膜过滤,得待测液。以Aglient Eclipse Plus C_(18)色谱柱为固定相,以5%(体积分数)甲醇溶液为流动相,在流量0.15 mL·min^(-1)下进行等度洗脱,电喷雾正离子(ESI^(+))模式和多反应监测(MRM)模式下测定,内标法定量。结果显示:丙烯酰胺标准曲线的线性范围为0.005~1.00 mg·L^(-1),检出限(3S/N)为0.0003 mg·L^(-1);对速溶咖啡和曲奇饼干样品进行3个浓度水平的加标回收试验,回收率为88.9%~111%,测定值的相对标准偏差(n=5)为2.5%~14%。

A method for the determination of acrylamide in instant coffee and cookies by UHPLC-MS/MS was developed.Instant coffee or cookies samples of 2.0 g was extracted twice with acetonitrile(10 mL×2)and degreased twice with hexane(10 mL×2).Acetonitrile phase of 10 mL was concentrated to nearly dryness under reducing pressure at 40℃.Water of 1 mL was added to the residue,and the solution obtained was filtered by 0.45μm water filtration membrane.Aglient EclipsePlus C_(18) column was used as stationary phase,and 5%(φ)methanol solution at a flow rate of 0.15 mL·min^(-1) was used as mobile phase for isocratic elution.Acrylamide was detected by ESI^(+)and MRM mode,and quantified by internal standard method.As shown by the results,linear range of the standard curve of acrylamide was 0.005-1.00 mg·L^(-1),with detection limit(3 S/N)of 0.0003 mg·L^(-1).Recovery test was made on the instant coffee and cookies samples at 3 concentration levels by standard addition method,giving results in the range of 88.9%-111%,with RSDs(n=5)of the determined values ranged from 2.5%to 14%.