食品科学 ›› 2008, Vol. 29 ›› Issue (4): 278-282.

• 分析检测 • 上一篇    下一篇

食品中丙烯酰胺测定的前处理条件和色谱条件优化

张辉珍, 马爱国, 孙永叶, 罗勇兵   

  1. 青岛大学医学院营养研究所; 青岛大学医学院营养研究所;
  • 出版日期:2008-04-15 发布日期:2011-08-24

Optimization of Pretreatment and Chromatographic Methods in Acrylamide Determination

 ZHANG  Hui-Zhen, MA  Ai-Guo, SUN  Yong-Ye, LUO  Yong-Bing   

  1. Institute of Nutrition, College of Medical, Qingdao University
  • Online:2008-04-15 Published:2011-08-24

摘要: 优化了食品中丙烯酰胺的高效液相色谱(HPLC-VWD)和气相色谱(elecfrochromismdevice,GC-μECD)分析方法。HPLC法采用C18(250×4.60mm,5μm)色谱柱,流动相为甲醇-0.02mol/L乙酸铵(体积比为5:95),流速0.6ml/min;检测波长205nm;GC法采用溴酸钾和溴化钾将丙烯酰胺的烯键加成为α,β-二溴丙酰胺后,用FFAP石英毛细管柱分离,电子捕获检测器定量测定。结果表明,两种方法均有良好的线性关系(r>0.99),HPLC方法的定量限为0.05mg/kg,平均加标回收率为86.3%~96.9%,相对标准偏差RSD为2.13%。GC-μECD法的定量限为0.02mg/kg,加标回收率为84.6%~98.5%,相对标准偏差RSD为4.36%。两种方法仪器设备易求,操作简便,回收率较高,精密度良好,用HPLC和GC两种方法测得的结果无显著性差异,均可用于油炸及焙烤类食品中丙烯酰胺的测定。

关键词: 丙烯酰胺, 高效液相色谱法, 气相色谱-电子捕获检测器, 衍生化

Abstract: A high performance liquid chromatographic (HPLC) method and a gas chromatographic method were optimized for the determination of acrylamide in food. HPLC method was used as follows: separation is carried out on a column of C18 (250 ×4.6 mm i.d 5μm) with methanol-0.02 mol/L ammonium acetate (5:95, V/V) as mobile phase, elution flow rate 0.6 ml/min and detection wavelength 205 nm. GC-μECD method was used as follows: KBrO3 and KBr are applied to derivate acrylamide into α,β-dibromopropionamide(2,3-DBPA)- 2-bromopenamide(2-BPA),while derivatives of acrylamide are separated by FFAP capillary column and determined by GC- μECD.The experimental results show a good linear relationship between the peak area and the concentration (r>0.99), where as the recoveries for acrylamide are resrectively 86.3 %~96.9 % for HPLC and 84.6 %~ 98.5 % for GC, and the relative standard deviation is respectively 2.13 % for HPLC and 4.36% for GC. The LOQ is respectively 0.05mg/kg for HPLC and 0.02 mg/kg for GC. The results show that the two methods have no notable diversity and both are simple, rapid, accurate and well suited for analysis of acrylamide in fried foods and baked foods as well.

Key words: acrylamide : HPLC; GC-&mu, ECD electrochromism device; derivate;