面粉中偶氮甲酰胺的高效液相色谱测定方法的优化

Optimization for determination of azodicarbonamide in flour by high performance liquid chromatography

目的建立面粉中偶氮甲酰胺测定的高效液相色谱法（HPLC）。方法以丙酮为提取液,样品提取液经离心浓缩后,用水复溶残渣,采用BDS HYPERSIL Cyano色谱柱（4.6 mm×250 mm,4.6μm）分离,二极管阵列检测器检测。结果在2～40μg/ml范围内,线性关系良好（r=0.999 8）,3个添加水平的回收率为74%～118%,相对标准偏差RSD〈5%。方法的定量限为3 mg/kg。结论本方法特异性强,前处理简单,适用于面粉中添加的偶氮甲酰胺快速筛查和定量。

Objective To establish a method of high performance liquid chromatography （ HPLC ） for the determination （ADA） of azodicarbonamide in flour. Methods Samples were extracted with acetone, then centrifuged and concentrated, the residue was dissolved with water. The injection was separated by cyano column and detected by photo-diode array. Results The method showed a good linearity in the range of 2-40μg/ml （r = 0. 999 8）. The recoveries of ADA from flour spiked at three levels were in the range of 74%-118% with the relative standard deviations less than 5%. The limit of quantification （LOQ） was 3 mg/kg. Conclusion This method could be used for screening and quantification of ADA in flour for its strong specificity and simple preparation.