丙烯酰胺中微量丙烯酸含量的高效液相色谱法分析

Determination of Trace Acrylic Acid in Acrylamide by High Performance Liquid Chromatography

建立了一种测定丙烯酰胺溶液中的微量丙烯酸含量的高效液相色谱法。采用常见的Agilent ZORBAX NH2液相色谱柱（5μm,4.6 mm×250 mm）,流动相为甲醇/水/磷酸盐体系,检测波长是205 nm,丙烯酸的保留时间在4.30 min左右,检出限为0.05 mg/L（S/N=3）,外标法定量测定。试样浓度在0.5 mg/L到20.0 mg/L范围内均有良好的线性关系,线性相关系数可达0.999 7;当试样加标浓度为1.0、5.0、10.0 mg/L时,加标回收率在87%~97%之间,RSD≤2.14%。此方法可成功应用于测量丙烯酰胺中微量的丙烯酸含量。

A high performance liquid chromatography （HPLC） method was established to determine trace acrylic acid content in acrylamide solution. Through external standard method, the quantity of acrylic acid was determined by utilizing Agilent ZORBAX NH2 liquid chromatographic column （5 μm, 4.6 mm× 250 mm）, mobile phase of methanol / water / phosphate system, 205 nm detection wavelength. The retention time of acrylic acid is at about 4.30 rain, and the detection limit is 0.05 mg/L （S/N=3）. As a result, when the sample concentration is between 0.5 mg/L to 20.0 mg/L, a good linear relationship can be obtained, and the linear correlation coefficient can reach to 0.999 7; When the external standard sample concentration is individually 1.0, 5.0, 10.0 mg/L, the recovery rate of standard sample is in the range of 87%-97%, RSD is less than or equal to 2.14%. This method can measure the trace content of acrylic acid in acrylamide.