采用HPLC-MS法检测中国传统发酵豆制品中丙烯酰胺含量。以ACQUITY UPLC C18色谱柱(210 mm×20 mm,1.7μm)为分离柱,流动相为0.1%甲酸水溶液和甲醇(体积比为99∶1),采用电喷雾正离子MRM模式检测和内标法定量(丙烯酰胺m/z:72.2∶55.0;内标13C3-丙烯酰胺m/z:74.79∶58.0)。该方法在0.01～1μg/mL有良好的线性关系(R=0.992 425),腐乳、豆豉以及豆酱的平均回收率分别为86.6%、91.7%和85.0%,RSD≦10%(n=5)。该方法灵敏度高,重现性好,适合于传统发酵豆制品中丙烯酰胺含量的测定。

A method for the determination of acrylamide in Chinese traditional fermented bean products by HPLC-MS was established.ACQUITY UPLC C18 column(210mm×20mm,1.7μm) was used for chromatographic separation,with elution of 0.1% formic acid in water and methanol(99∶ 1 by volume).Determination was performed by using electrospray ionixation(ESI+) and multi-reaction monitoring(MRM).Internal standard method was applied to quantify.The m/z for acrylamide was 72.2∶ 55,the m/z for 13C3-acrylamide was 74.79∶ 58.0.The calibration linear range of acrylamide was from 0.01~1μg/mL with correlation coefficient of 0.992425.The mean recovery of fermented bean curd,fermented black bean and soybean paste were 86.6%,91.7% and 85.0%,the relative standard deviation was lower than 10%(n=5).This method was highly sensitive and well repeatable,and was suitable for quantifying the contents of acrylamide in Chinese traditional fermented bean products.