建立了气相色谱-质谱(GC-MS)定量测定食品中丙烯酰胺含量的分析方法.选择<'13>C<,3>-丙烯酰胺作为内标物.通过超纯水提取食品中的丙烯酰胺,经正已烷脱脂两次后,在酸性条件下选用溴化钾/溴酸钾为衍生剂进行衍生化反应,再采用乙酸乙酯进行液-液萃取两次,最后用三乙胺将丙烯酰胺转化为更稳定的产物2-溴丙烯酰胺,利用质谱检测器在选择离子扫描模式下测定2-溴丙烯酰胺.该方法在0.05～2.00 mg/kg范围具有良好的线性(r<'2>=0.999 5);检出限和定量限分别达到3 μg/kg和7 μg/kg;回收率范围为62.7%～65.5%.通过与前期建立的液相色谱-串联质谱(HPLC-MS/MS)方法进行对比,该法在薯片和面包样品中丙烯酰胺的检测结果略偏高,是一种可以用于常见食品中丙烯酰胺含量测定的分析方法.%The quantification of acrylamide in foods was investigated by gas chromatographymass spectrometry (GC-MS).In this method, 13C3-acrylamide was used as an internal standard.The samples were homogenized, defatted with hexane and extracted with ethyl acetate for twice.The derivatization of acrylamide into 2-bromopropenamide (2-BPA) was done using potassium bromide/potassium bromate at 4 ℃ for 90 min.Selective ion monitoring mode was chosen to monitor objective chromatography.This method had a good linearity between 0.05 -2.00 mg/kg (r2 = 0.999 5 ), and the limits of detection and quantification were 3 μg/kg and 7μg/kg, respectively.The recoveries of acrylamide were in the range of 62.7％ - 65.5％.In order to confirm this GC-MS method, the acrylamide in foods was also determined by high performance liquid chromatography coupled to quadrupole tandem mass spectrometry (HPLC-MS/MS), which had been proved in our laboratory.The concentrations of acrylamide in the samples quantified by GC-MS were slightly higher than those detected by HPLC-MS/MS.This method can be used to quantify acrylamide in normal foods.
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