亲水作用高效液相色谱-串联质谱法测定薯片及饼干中丙烯酰胺的含量

Determination of acrylamide in potato chips and biscuits by hydrophilic interaction-high performance liquid chromatography-tandem mass spectrometry

目的建立亲水作用高效液相色谱-串联质谱法测定薯片及饼干中丙烯酰胺含量的分析方法。方法薯片及饼干经超纯水提取,正己烷除脂,Cleanert■ACA固相萃取柱净化,BEH Amide色谱柱(2.1mm×100mm,1.7μm)分离,并以0.1%(V:V)甲酸水-乙腈溶液=2:8(V:V)为流动相,电喷雾正离子模式电离,多反应监测模式检测,内标法定量。结果丙烯酰胺在5~2000μg/L范围内线性关系良好,相关系数大于0.999。方法的检出限(S/N>3)和定量限(S/N>10)分别为3μg/kg和10μg/kg。在不同基质中,丙烯酰胺在20、200、1000μg/kg的添加水平下平均加标回收率为91.5%~98.2%,相对标准偏差为2.71%~4.82%。结论此方法具有准确度好、灵敏度高等特点,适用于薯片及饼干中丙烯酰胺的测定。

Objective To establish a method for determination of acrylamide in potato chips and biscuits by hydrophilic interaction-high performance liquid chromatography-tandem mass spectrometry.Methods Acrylamide in potato chips and biscuits was extracted with ultrapure water and purified with hexane and Cleanert■ ACA solid phase extraction.The separation was performed on BEH Amide chromatographic column(2.1 mm×100 mm, 1.7 μm)with the mobile phase of 0.1% formic acid solution-acetonitrile(2:8, V:V).It was monitored by positive electrospray ionization(ESI+) and multi reaction mode, and quantified by internal standard method.Results Acrylamide had good linear relationship in the range of 5-2000 g/L, and the correlation coefficients were greater than 0.999.The limit of detection(S/N>3) and limit of quantitative(S/N>10) were 3 μg/kg and 10 μg/kg, respectively.In different substrates, the recoveries at 3 spiked levels(20, 200 and 1000 μg/kg) were 91.5%-98.2%, with the relative standard deviations of 2.71%-4.82%.Conclusion This method is accurate and sensitive, which is suitable for determination of acrylamide in potato chips and biscuits.