建立了方便面中丙烯酰胺的液相色谱-串联质谱分析方法。样品用水提取，酶解，净化。以水（0.1%甲酸）:乙腈=90:10(V/V)为流动相经反相色谱柱分离后，采用液相色谱串联质谱多反应监测正离子模式检测，丙烯酰胺定性定量离子对为m/z 72.10/55.00，同位素内标物定性定量离子对为75.00/58.00。空白样品及其添加实验结果表明，特征离子相对强度比值稳定，无基质干扰，结合保留时间可实现准确的定性定量，方法检出限为25 μg/kg (S/N=3)，样本添加水平在5~200 μg/kg时，平均回收率为68.1%~90.1%，相对偏差(n=6)为4.3%~6.1%。该方法前处理简单、回收率高、精密度好，可满足方便面中丙烯酰胺的确证分析要求。

A novel method for the determination of acrylamide in fried instant noodles with HPLC/MS/MS was established. Acrylamide was extracted by water from the hydrolyzed fried instant noodle by amylase, separated by RP-HPLC using the mixture of 0.1%HCOOH solution and CH3CN (90:10, v/v) as mobile phase and then detected by the positive electrospray ionization utilizing multiple reaction monitoring of one parent-daughter ion pair (m/z 72.10/55.00) and the isotope internal standard for qualitative and quantitative ion pair (m/z 75.00/58.00) Results showed that the relative intensity of the acrylamide identification ion pairs in instant noodles was stable and no matrix interference with these diagnostic ion pairs was found. The method could be used for accurate qualitative and quantitative analysis of acrylamide with the LOD (S/N=3) of 25 μg/kg. Within the range of 5~200 μg/kg, the average recoveries were 68.1%~90.1% with RSD (n=6) values between 4.3% and 6.1%. This method was simple, precise and had high recoveries, which could be used for the determination of acrylamide in fried instant noodle samples.

粤港关键领域重点突破招标项目2005A20501003