摘要
建立了以离子液体作反相高效液相色谱流动相添加剂分离测定邻苯二胺、苯胺和对甲苯胺3种芳香胺的方法。实验以C18反相色谱柱为分离柱,采用紫外检测方法,考察了检测波长、甲醇含量、咪唑离子液体烷基链长度、离子液体溶液浓度等条件对分离和测定的影响,并与其它分离测定芳香胺的方法进行了比较。优化的色谱条件为:以甲醇/1-丁基-3-甲基咪唑四氟硼酸盐水溶液(3.0mmol/L,乙酸调节pH 3.5)=30/70(V/V)为流动相;检测波长254 nm;流速1.0mL/min;柱温30℃。在此条件下,3种芳香胺达到基线分离,在6.5 min之内分离完全;在1～40 mg/L范围内,线性回归方程的相关系数达到0.99以上;检出限为0.07～0.41 mg/L。将本方法应用于废水的测定,加标回收率在92.3%～96.7%之间,相对标准偏差小于3.5%。
A reversed-phase high performance liquid chromatographic method with ionic liquids as mobile phase additives for separation of three kinds of aromatic amines including o-phenylenediamine,aniline and p-toluidine was developed.The chromatographic separation of aromatic amines was performed on a RP-C18 column.The detection of aromatic amines was carried out by an ultraviolet（UV） detector.The effects of detection wavelength,methanol content,length of alkyl chain on different imidazolium ionic liquids and concentration of ionic liquids on the separation and determination of aromatic amines were investigated.The comparison of three different mobile phases was performed.The optimum chromatographic conditions were confirmed as follow： methanol/1-butyl-3-methylimidazolium tetrafluoroborate aqueous solution（3.0 mmol/L,pH 3.5 adjusted with acetic acid）=30/70（V/V） as mobile phase,UV detection wavelength 254 nm,flow rate 1.0 mL/min,column temperature 30 ℃.The three kinds of aromatic amines were successfully separated within 6.5 min under the optimal conditions.The calibration curves showed good linearity over the tested range from 1 to 40 mg/Lfor aromatic amines with correlation coefficients of 0.99.The detection limits of aromatic amines were 0.07-0.41 mg/L.The method has been applied to analyze the waste water with spiked recoveries of 92.3%-96.7% and the relative standard deviation was less than 3.5%.The method was simple,accurate and reliable.
出处
《分析试验室》
CAS
CSCD
北大核心
2012年第5期47-51,共5页
Chinese Journal of Analysis Laboratory
基金
黑龙江省自然科学基金项目(B200909)
黑龙江省高校科技创新团队建设计划项目(2011TD010)资助
关键词
离子液体
高效液相色谱法
芳香胺
紫外检测
废水
Ionic liquid
High performance liquid chromatography
Aromatic amine
Ultraviolet detection
Waste water
