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.
出处
《分析试验室》
CAS
CSCD
北大核心
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
关键词
高效液相色谱
对位酯
对氯苯胺
质量控制
High performance liquid chromatography Para-ester P-chloroaniline Quality control
