摘要
建立了超高效液相色谱法测定环境水样中甲酰胺、N-甲基甲酰胺、N-甲基乙酰胺、N,N-二甲基甲酰胺(DMF)和N,N-二甲基乙酰胺(DMAC)等酰胺类化合物含量的方法。环境水样经活性炭固相萃取柱富集净化,上样1.0~50.0 mL,用3.0 mL乙腈洗脱,洗脱液经过浓缩、溶剂置换后进行色谱分析。采用Athena C18-WP液相色谱柱,选择乙腈:水(5:95,V/V)为流动相,设定流速为1.0 mL/min,柱温为30℃,紫外检测波长为195 nm。实验考察了固相萃取柱种类、样品上样量、洗脱溶剂用量、淋洗溶剂用量等对分析结果的影响。5种酰胺类化合物在最终优化条件下能在15 min内实现分离,在0.4~10.0 mg/L范围内呈良好线性关系(相关系数大于0.99),检出限为2×10-4~0.02 mg/L,方法加标回收率81.6%~100.6%,精密度为0.37%~0.94%。本方法操作简便、快速准确,可同时测定环境水样中的酰胺类化合物。
A method for the determination of formamide(FM),N-methylformamide(NMF),N-methylacetamide(NMAC),N,N-dimethylformamide(DMF)and N,N-dimethylacetamide(DMAC)in environmental water samples by ultra performance liquid chromatography was established.A cartridge containing carbon black was used for enrichment and cleanup of environmental water by solid phase extraction(SPE).The sample loaded was 1.0-50.0 mL,and then eluted with 3.0 mL acetonitrile,the elution was injected and analyzed by HPLC after concentration and solvent exchange.Athena C18-WP column and mobile phase of acetonitrile:water(5:95,V/V)were used.The flow rate was 1.0 mL/min,the column temperature was 30℃,and the UV detection wavelength was 195 nm.The effects of the type of solid phase extraction column,the amount of sample loading,rinsing solvent and elution solvent on the analysis result were investigated.The results showed that,five amide compounds were determined within 15 min under the optimized conditions.The calibration curves were linear in range of 0.4~10.0 mg/L with correlation coefficients of 0.99.The detectable concentration(LOD)was 2×10-4~0.02 mg/L,and the average recoveries were81.6%~100.6%,with the precision of 0.37%~0.94%.The method is simple,rapid and accurate,and can simultaneously determine amide compounds in environmental water samples.
作者
罗青青
牛禾
严朝朝
章心怡
袁继委
余彬彬
LUO Qing-qing;NIU He;YAN Zhao-zhao;ZHANG Xin-yi;YUAN Ji-wei;YU Bin-bin(School of Pharmaceutical and Materials Engineering,Taizhou University,Zhejiang Taizhou 318000,China;Taizhou Environmental Monitoring Center,Zhejiang Taizhou 318000,China)
出处
《当代化工》
CAS
2020年第3期741-744,共4页
Contemporary Chemical Industry
基金
浙江省化学工程与技术一流学科(台州学院)开放基金
国家大学生创新创业训练计划项目(201910350011).
