固相萃取-亲水相互作用液相色谱法同时测定环境水样中3种酰胺类化合物

Determination of Three Amide Compounds in Environmental Water by Solid Phase Extraction Coupled with Hydrophilic Interaction Liquid Chromatography

基于亲水相互作用液相色谱(Hydrophilic Interaction Liquid Chromatography,HILIC)技术,建立了同时测定环境水样中丙烯酰胺、N,N-二甲基甲酰胺和N,N-二甲基乙酰胺的液相色谱分析方法。水样采用石墨化碳黑固相萃取柱净化,上样1.0 mL,并最终用1.0 mL乙腈洗脱,洗脱液进样色谱分析。选择Waters HILIC色谱柱,以乙腈/水作为流动相,等度洗脱,二极管阵列检测器200 nm条件下检测。在优化的分析条件下,3种酰胺类化合物在11 min内实现基线分离。所有目标化合物浓度在0.05～100 mg/L范围内线性良好,相关系数均大于0.9999;检出限达0.01 mg/L。加标回收率为84.1%～106%;相对标准偏差1.8%～10.4%。本方法具有简便快捷、灵敏准确等特点,能够满足环境水样中痕量酰胺类污染物检测的要求。

A simple hydrophilic interaction liquid chromatographic（HILIC） method for the determination of acrylamide（AA）,N,N-dimethylformamide（DMF）,and N,N-dimethylacetamide（DMAC） in environmental water was developed.A cartridge containing graphitized carbon black was used for solid phase extraction（SPE） of the compounds in environmental water,the sample loaded was 1.0 mL,and then eluted with 1.0 mL acetonitrile,the elution was introduced into the instrument and determined by HPLC coupled with photo-diode array detector（PDA） at 200 nm.A good baseline separation of target compounds was obtained in 11 minutes under the optimum condition of determination.The calibration curves of 3 amides were linear in the concentration range of 0.05-100 mg/L with correlation coefficients of 0.9999.Overall recoveries were good（84.1%-106%）,and the relative standard deviations ranged from 1.8% to 10.4% for the target compounds.The minimum detectable concentrations were 0.01 mg/L.This established method is convenient,sensitive and accurate,and was suitable for the routine detection of trace amide contaminants in environmental water.