液相色谱-串联质谱法测定黑糖中丙烯酰胺和天冬酰胺

Determination of acrylamide and L-asparagine in black sugar products by liquid chromatography-tandem mass spectrometry

目的建立同时检测黑糖产品中丙烯酰胺和天冬酰胺的液相色谱-串联质谱法(liquid chromat ography-tandem mass spectrometry,LC-MS/MS)。方法黑糖产品样品经纯水提取净化后直接测定,采用含有5mmol/L的乙酸铵、0.1%的甲酸水(A)和乙腈(B)作为流动相进行梯度洗脱,质谱采用多反应监测模式监测定性和定量离子。结果丙烯酰胺和天冬酰胺在0.1、0.2、0.5 mg/L 3个添加浓度上回收率范围为93.5%~108.0%,相对标准偏差为1.4%~5.4%,检出限分别为0.01、0.005 mg/L。结论本方法前处理操作快速简单,可重复性好,满足国内外对黑糖产品中丙烯酰胺和天冬酰胺的快速、准确的检测要求,适合大量样品的准确定量和定性分析。

Objective To establish a method for the determination of acrylamide and L-asparagine in black sugar products by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The black sugar product samples were extracted and purified by pure water and directly determined.The mobile phase was gradient elution with 5 mmol/L ammonium acetate,0.1%formic acid water(A)and acetonitrile(B).The qualitative and quantitative ions were monitored by mass spectrometry using multiresponse monitoring model.Results The recoveries of acrylamide and L-asparagine at 0.1,0.2,0.5 mg/L were 93.5%-108.0%,and the relative standard deviations were 1.4%-5.4%.The limits of detection were 0.01,0.005 mg/L Conclusion This method is simple and fast,and has good repeatability.It can meet the requirements of rapid and accurate detection of acrylamide and L-asparagine in black sugar products at home and abroad,and is suitable for accurate quantitative and qualitative analysis of a large number of samples.