高效液相色谱法测定水中痕量丙烯酰胺

摘要

建立旋转蒸发浓缩周相萃取与高效液相联用测定水中痕量丙烯酰胺的方法.水样经旋转蒸发浓缩活性炭固相萃取柱净化后进行高效液相色谱分析,流动相为甲醇:水(10:90).流速为0.8 mL/min,进样量为20μL,检测波长为210 nm,丙烯酰胺标准溶液介质为超纯水.试验表明:在同等条件下采用超纯水配制标准丙烯酰胺溶液进行高效液相测定的灵敏度比用甲醇配制的高5倍,线性范围为5～250μg/L,r=0.999 8;在浓缩100倍的条件,丙烯酰胺回收率为83%～95%,水样最低检测限为50 ng/L.该方法经济、简单、灵敏、准确,可向常规实验室推广.%Established a rotary evaporation - solid phase extraction - high performance liquid chromatography method for the determination of acrylamide in water.Water samples by rotary evaporation, purified by activated carbon SPE column and then analyzed by HPLC.The mobile phase was 10 ％ methanol-water solution, the flow rate was 0.8 mL/min, the volume of injection was 20 μL,the detection wavelength was 210 nm and acrylamide standard solution medium was ultra-pure water.Results show that: Under the same conditions, HPLC determination of acrylamide standard solution in ultra-pure water more sensitive than the configured with methanol 5 times.The linearity range of the method was 5～250 μg/L with correlation coefficient of 0.999 8.Concentrated 100 times in the conditions, acrylamide recoveries ranged from 83 ％ to 95 ％.The detection limit of the water sample was 50 ng/L.This method is cheap, convenient, sensitive and accurate and it can be applied in general laboratories.