论文部分内容阅读
目的建立面粉及其制品中偶氮甲酰胺的高效液相色谱检测方法。方法样品采用丙酮—二甲基甲酰胺(95∶5,v/v)超声提取,经乙腈饱和的正己烷脱脂,注入高效液相色谱后,以20 mmol/L乙酸铵与乙腈(均含5%二甲基甲酰胺)为流动相,等度洗脱,经Waters XBridge BEH Amide(3.5μm,4.6 mm×150 mm)色谱柱分离,二极管阵列检测器245 nm检测,外标法定量。结果方法的线性范围为1.0~100.0 mg/L,线性相关系数r为0.999 9;在面粉、馒头、面包、油条和面条5种基质中高中低3个浓度水平的平均加标回收率为90.20%~99.74%,相对标准偏差(RSD)2.82%~6.31%;方法定量限(LOQ)为0.5 mg/kg。结论该方法操作简单、灵敏快速、准确可靠,适用于面粉及其制品中偶氮甲酰胺含量的测定。
Objective To establish a HPLC method for the determination of azodicarbonamide in flour and its products. Methods The samples were extracted with acetone-dimethylformamide (95: 5, v / v) and degreased by n-hexane saturated with acetonitrile. After injecting high performance liquid chromatography (HPLC), the samples were eluted with 20 mmol / L ammonium acetate and acetonitrile % Dimethylformamide) as the mobile phase, isocratic elution, separated by Waters XBridge BEH Amide (3.5 μm, 4.6 mm × 150 mm) column, detected by a diode array detector at 245 nm, and quantified by external standard method. Results The linear range of the method was 1.0-100.0 mg / L and the linear correlation coefficient was 0.999 9. The average recoveries for the three medium, medium and low concentrations of flour, bread, bread, fried dough sticks and noodles were 90.20% ~ 99.74%, relative standard deviation (RSD) 2.82% ~ 6.31%. The limit of quantification (LOQ) was 0.5 mg / kg. Conclusion The method is simple, sensitive and rapid, accurate and reliable, suitable for the determination of azodicarbonamide in flour and its products.