小麦粉及其制品中偶氮甲酰胺的检测方法研究

Determination of azodicarbonamide in wheat flour and its preparation

建立了液相色谱法测定小麦粉及其制品中偶氮甲酰胺含量的方法。样品用丙酮提取，提取液氮吹浓缩后用水定容，并用正己烷脱脂。样液供高效液相色谱仪测定，采用色谱柱为ZORBAXSB—CN（250mm×4．6mm，5μm），以体积比为10％的甲醇和90％的20mmol／L乙酸铵溶液为流动相，流速为O．8mL／min，柱温为30℃，进样量为20止，最大吸收波长为245nm，外标法定量。本方法偶氮甲酰胺峰面积对浓度在0～50mg／L范围内线性关系良好，相关系数r=0．9999，回收率89％～95％，相对标准偏差小于5％。方法准确可靠，定量限1．0mg／kg，检出限0．3mg／kg，可作为小麦粉及其制品中偶氮甲酰胺含量检测的有效定量方法。该方法的建立为小麦粉及其制品中偶氮甲酰胺的检测标准的制定提供了参考，同时对市场上相关产品的监督管理提供了技术支撑。

A method of measuring azodicarbonamide （ADA） in wheat flour and its preparation based on HPLC was presented. The ADA in wheat flour and its preparation was extracted with acetone, concentrated under nitrogen and diluted with water. After removed the lipid by hexane, the extract was analyzed by HPLC. Chromatagraphy was conducted on a ZORBAX SB-CN （250mm × 4.6mm, 5lxm） at 30 ℃ and 275nm, The mobile phase was methanol ： 20mmol/L acetate solution=10 ： 90 （v ： v） at a flow rate of 0.8 ml/minl.The calibration curve was linear in the range of 0 - 50mg/L （r=019999）, The recovery was between 89% and 95% and RSD less than 5%.The method was reliable , the quantification limit was 1.0mg/kg, the detection limit was 0.3mg/kg. It was a very effective method in measuring the ADA in wheat flour and its preparation. The method provides a reference for the detection of the wheat flour and its products, at the same time provides technical support for the supervision and management on the market related products.