高效液相色谱串联质谱法测定食糖中丙烯酰胺

摘要

建立了食糖中丙烯酰胺的高效液相色谱串联质谱(HPLC-MS/MS)检测方法。食糖样品用甲醇提取后，上清液浓缩，以流动相复溶，采用XBridgeTM Amide(3.5μm，4.6×150 mm)柱，以甲醇和0.1%甲酸水为流动相进行洗脱，电喷雾质谱正离子模式(ESI+)，多反应监测(MRM)检测，同位素内标法定量。该方法在20～2000μg/L线性良好(r =0.9991），检出限为6.0μg/L。分别在样品中添加标准物质50、100、200μg/kg进行回收率实验，方法的回收率范围为101%～109%，相对标准偏差为5.3%～8.3%(n=6)。该方法样品前处理简单、快速，分析时间短，灵敏度、准确度和精密度均满足食糖中丙烯酰胺的检测要求。%A method was developed for the determination of acrylamide in sugar by High Performance Liquid Chromatography Tandem Mass Spectrometry (HPLC-MS/MS). The sugar samples were extracted by methanol, and then centrifugated. Chromatographic separation was achieved on XBridgeTM Amide column (3.5 μm, 4.6×150 mm). The mobile phase consisted of 0.1% aqueous formic acid solution and methanol, then analyzed by using HPLC-MS/MS in multiple reaction monitoring (MRM) mode via positive electrospray ionization. Isotope internal standards were used for quantitative analysis. External standard method was used to determine the residue contents with a good linear relationship (r=0.9991). The limits of quantification (LOQ) was 6.0 μg/kg. The recoveries of acrylamide at 3 levels of 50, 100, and 200 μg/kg were from 101% to 109% with the relative standard deviations (RSDs) of 5.3%-8.3% (n=6) in sugar. The method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the residue analysis. This developed procedure is suitable for the determination of acrylamide in sugar.