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

中文关键词:  丙烯酰胺  亲水作用  高效液相色谱-串联质谱法  薯片及饼干

英文关键词:acrylamide  hydrophilic interaction  high performance liquid chromatography-tandem mass spectrometry  potato chips and biscuits

中文摘要:

      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(2.1 mm×100 mm, 1.7 μm)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5~2000 μg/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3 μg/kg和10 μg/kg。在不同基质中, 丙烯酰胺在20、200、1000 μg/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。

英文摘要:

      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.