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文章建立了溴化衍生-液液小体积萃取-气相色谱法-电子捕获检测器(GC-ECD)测定水中丙烯酰胺的方法。优化了前处理步骤,缩短了样品的处理时间,减少了试剂和样品的使用量。取20 mL水样,分别加入H2SO4、KBrO3、KBr,4℃下反应至少30 min,丙烯酰胺与新生溴反应生成2,3-二溴丙酰胺。加入Na2S2O3去除多余的溴,加无水硫酸钠于室温下溶解盐析,用2.0 mL乙酸乙酯萃取,取上层萃取液GC-ECD分析。用衍生物2,3-二溴丙酰胺的响应峰面积对水中丙烯酰胺的质量浓度绘制工作曲线,相关系数达到0.999 47。方法适用于饮用水、地表水中丙烯酰胺的测定,检出限可达到0.026μg/L,相对标准偏差RSD为2.70%,加标回收率为80.67%~100.43%。
A method for the determination of acrylamide in water by brominated derivative-liquid-liquid small-volume extraction-gas chromatography-electron capture detector (GC-ECD) was established. Optimize the pre-treatment steps, shorten the sample processing time, reducing the reagents and sample usage. Take 20 mL of water sample, add H2SO4, KBrO3, KBr respectively, and react at 4 ℃ for at least 30 min. Acrylamide reacts with newborn bromine to produce 2,3-dibromopropionamide. Add Na2S2O3 to remove excess bromine, add anhydrous sodium sulfate, dissolve salting out at room temperature, extract with 2.0 mL of ethyl acetate and take GC-ECD analysis of the upper extract. The working curve of the mass concentration of acrylamide in water was plotted with the peak area of the derivative 2,3-dibromopropionamide, and the correlation coefficient reached 0.999 47. The method was applied to the determination of acrylamide in drinking water and surface water. The detection limit was 0.026 μg / L, RSD was 2.70% and the recoveries were 80.67% -100.43%.