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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%)。
A method for the determination of p-chloroaniline in para-ester and its related impurities in industrial para-esters was established by reversed-phase high performance liquid chromatography. Chromatographic conditions were optimized on a C 18 column (4.6 × 150 mm, 5 μm) by examining the effect of mobile phase species, organic modifier ratio, p H etc. on retention. A reversed-phase high performance liquid chromatography (RP-HPLC) was developed for the simultaneous determination of p-chloro-p-chloroaniline and p-chloroaniline. The RP-HPLC method was developed for the rapid determination of p-chloroaniline. Reversed-phase high performance liquid chromatography can be used for the qualitative analysis of related impurities in para-ester by liquid chromatography-mass spectrometry. In reversed-phase ion-pair high performance liquid chromatography with simultaneous determination of para-ester and p-chloroaniline, the para-chloro-aniline and p-chloroaniline were found to be 0.78-1000.0 μg / mL (r = 0.9997) and 0.31-20.00 μg (r = 0.9999). The average recoveries (n = 3) were 100.1% (RSD = 0.62%) and 100.8% (RSD = 1.3% (R = 0.9995). The average recoveries (n = 3) were 102.0% (RSD = 0.43% ).