Zhu Yonghong, Li Genrong, Duan Yunpeng, Chen Shiqi, Zhang Chun, Li Yanfei
Quality Supervision and Inspection Center of Food, Chongqing Academy of Metrology and Quality Inspection, Chongqing 400 020, China.
Quality Supervision and Inspection Center of Food, Chongqing Academy of Metrology and Quality Inspection, Chongqing 400 020, China.
Food Chem. 2008 Aug 15;109(4):899-908. doi: 10.1016/j.foodchem.2008.01.020. Epub 2008 Jan 20.
A gas chromatography electron capture detector (GC-ECD) using the standard addition method was developed for the determination of acrylamide in heat-processed foods. The method entails extraction of acrylamide with water, filtration, defatting with n-hexane, derivatization with hydrobromic acid and saturated bromine-water, and liquid-liquid extraction with ethyl acetate. The sample pretreatment required no SPE clean-up and concentration steps prior to injection. The final extract was analyzed by GC-ECD. The chromatographic analysis was performed on polar columns, e.g. Supelcowax-10 capillary column, and good retention and peak response of the analyte were achieved under the optimal conditions. The qualification of the analyte was by identifying the peak with same retention time as standard compound 2,3-DBPA and confirmed by GC-MS. GC-MS analysis confirmed that 2,3-DBPA was converted to 2-BPA nearly completely on the polar capillary column, whether or not treated with triethylamine. A four-point standard addition protocol was used to quantify acrylamide in food samples. The limit of detection (LOD) was estimated to be 0.6μg/kg on the basis of ECD technique. Validation and quantification results demonstrated that the method should be regarded as a low-cost, convenient, and reliable alternative for conventional investigation of acrylamide.
建立了一种采用标准加入法的气相色谱电子捕获检测器（GC-ECD），用于测定热处理食品中的丙烯酰胺。该方法包括用水提取丙烯酰胺、过滤、用正己烷脱脂、用氢溴酸和饱和溴水衍生化以及用乙酸乙酯进行液-液萃取。样品预处理在进样前无需固相萃取净化和浓缩步骤。最终提取物通过GC-ECD进行分析。色谱分析在极性柱上进行，例如Supelcowax-10毛细管柱，在最佳条件下实现了分析物的良好保留和峰响应。分析物的定性是通过鉴定与标准化合物2,3-DBPA保留时间相同的峰，并通过GC-MS进行确认。GC-MS分析证实，无论是否用三乙胺处理，2,3-DBPA在极性毛细管柱上几乎完全转化为2-BPA。采用四点标准加入方案对食品样品中的丙烯酰胺进行定量。基于ECD技术，检测限（LOD）估计为0.6μg/kg。验证和定量结果表明，该方法应被视为传统丙烯酰胺检测的一种低成本、方便且可靠的替代方法。
