高效液相色谱法测定面粉中偶氮甲酰胺的含量

Determination of azodicarbonamide in flour by high performance liquid chromatography

摘要:

目的：建立面粉中偶氮甲酰胺（azodicarbonamide，ADC）的高效液相色谱检测方法。方法：样品经丙酮提取，正己烷脱脂，进入高效液相色谱后采用Eclipse XDB-CN柱（250 mm×4.6 mm，5 μm）进行分离，以乙腈-20 mmol/L乙酸铵为流动相进行梯度洗脱，二极管阵列检测器检测波长为245 nm。结果：ADC在1.0～90.0 mg/kg范围内线性关系良好，相关系数（r）大于0.99，定量限为5 mg/kg（S/N≥10），在5.0、10.0、45.0 mg/kg 3个添加水平下回收率在68.6%～116.9%之间，相对标准偏差均小于7.0 %。结论：建立的面粉中ADC液相色谱方法简单快捷，准确可靠，适用于面粉中ADC的测定。

Abstract:

Objective：To develop an analytical method based on high performance liquid chromatography（HPLC） for the determination of azodicarbonamide（ADC） in flour. Methods：Samples were extracted with acetone，degreased with n-hexane，then separated with a agilent Eclipse XDB-CN column（250 mm× 4.6 mm，5 μm） using acetonitrile-ammonium acetate（20 mmol/L） as mobile phase with a gradient elution program and were detected with diode array detector with the wavelength of 245 nm. Results：ADC had a good linear relationship within the range of 1.0-90.0 mg/kg；the correlation coefficient was higher than 0.99 and the limit of quantification（S/N≥10） was 5.0 mg/kg. Average recoveries of ADC at spiking levels of 5.0，10.0，45.0 mg/kg were ranged from 68.6% to 116.9% and relative standard deviations were less than 7.0%. Conclusions：The method developed is simple，rapid，accurate and reliable；it can be used for the determination of ADC in flour.