反相高效液相色谱法测定对位酯工业品中的对位酯和对氯苯胺  

Determination of para-ester and p-chloroaniline in industrial para-ester by RP-HPLC

作　　者：韦兰春[1] 乔俊琴[1] 练鸿振[1] 

机构地区：[1]生命分析国家重点实验室南京大学化学化工学院和现代分析中心,南京210093

出　　处：《分析试验室》2016年第5期526-531,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(21275069;21577057);南京大学分析测试基金资助

摘　　要：建立了利用反相高效液相色谱测定工业对位酯中对位酯及其相关杂质对氯苯胺含量的方法。在C_（18）色谱柱（4.6×150 mm,5μm）上通过考察流动相种类、有机调节剂比例、p H等对保留的影响来优化色谱条件。分别建立了同时测定对位酯和对氯苯胺的反相离子对高效液相色谱法、快速测定对氯苯胺的反相高效液相色谱法,并建立了进一步分离对位酯中其他相关杂质的反相高效液相色谱法,可用于对位酯中相关杂质的液相色谱-质谱联用定性分析。在建立的同时测定对位酯和对氯苯胺的反相离子对高效液相色谱法中,对位酯和对氯苯胺分别在0.78-1000.0μg/m L（r=0.9997）和0.31-20.00μg/m L（r=0.9999）的浓度范围内成线性关系,平均回收率（n=3）分别为100.1%（RSD=0.62%）和100.8%（RSD=1.3%）;在快速测定对氯苯胺的反相高效液相色谱法中,对氯苯胺在0.25-200.0μg/m L（r=0.9995）的浓度范围内成线性关系,平均回收率（n=3）为102.0%（RSD=0.43%）。The analytical methods were proposed for the determination of para-ester and p-chloroaniline in industrial para-ester by reversed phase high performance liquid chromatography（ RP-HPLC）. Performance was carried out on a C_（18）column（ 4. 6 mm × 150 mm,5 μm）,and the chromatographic conditions were optimized by investigating the influences of mobile phase kind,organic modifier content,p H,and etc,on the retention of the analytes. Three methods were established respectively,including simultaneous determination of para-ester and its related impurities p-chloroaniline by reversed phase ion pair liquid chromatography（ RP-IP-HPLC）,rapid determination of p-chloroaniline by RP-HPLC,and a RP-HPLC method for the further separation of other impurities in para-ester which is suitable for the identification of the relative impurities by LC-MS.

关 键 词：高效液相色谱 对位酯 对氯苯胺 质量控制 

分 类 号：TQ61[化学工程—精细化工]