二极管阵列检测高效液相色谱法测定食品中丙烯酰胺的研究

Determination of acrylamide in food by using diode array detector and high performance liquid chromatography

目的研究检测食品中致癌物丙烯酰胺的固相萃取-二极管阵列检测-反相高效液相色谱测定方法,以用于各种食品中丙烯酰胺的测定。方法用水提取食品中丙烯酰胺,采用C18固相萃取小柱对样品液进行纯化,用高效液相色谱分离后以二极管阵列检测器测定其含量。色谱条件:AglientXDB反相C18柱(20cm×4.6mm,5μm);流动相为甲醇:水(体积比5:95),流速0.8ml/min,柱温40℃,DAD扫描波长范围190～370nm,检测波长210nm;进样量5μl。结果丙烯酰胺在0.1～10mg/L浓度范围内线性良好,相关系数r=0.999;方法检出限为10ng/g,回收率大于95%,精密度为5.34%(低浓度)、3.40%(中等浓度)和4.30%(高浓度)。结论建立的二极管阵列检测高效液相色谱法测定食品中丙烯酰胺满足痕量分析要求,并具有操作简单、干扰少、快速、准确可靠等特点,可用于我国食品中丙烯酰胺状况调查。

Objective To explore the method for determination of aerylamide in food by solid phase extraction and diode array detector and high performance liquid chromatography （SPE-DAD-HPLC）. Methods The aerylamide in food was extracted by water, and purified by solid phase extraction, then detected by diode array detector of high performance liquid chromatography. The HPLC system consisted of Aglient XDB C18 column （20cm×4.6mm,5μm）, mobile phase of methanol：water （5：95）, column temperature 40℃, wavelength of scan from 190nm to 370nm, DAD detector at 210nm. Results The linear ranges of determination of acrylamide was 0.1～10mg/L （r=0.999）. The detection limit of the method was 10ng/g. The roeovefiys was over 95.0%, RSD was 5.34%（low concentration）, 3.40% （middle concentration） and 4.30% （high concentration）. Conclusion The method for determination of aerylamide in foods by SPE - DAD - HPLC with little interference, easy and accurate. It can be used for determination of aerylamide in food.