高效液相色谱法测定AMPS/AM二元共聚物中残余微量单体含量

摘要

A high performance liquid chromatography for the analysis of residual monomers,2-acrylamido-2-methyl propane sulfonic acid(AMPS) and acrylamide(AM),in AM/AMPS copolymer was established.In order to reduce the viscosity of samples,the mixture of isopropanol and ethanol was used as the extractant to extract AMPS and AM from the aqueous solution of AM/AMPS copolymer.The effects of the wavelength and proportion of mobile phases on the separation were investigated to choose the optimal analysis conditions.The results show that the optimal conditions are as follow:chromatographic column ZORBAX SB-C18(4.0 mm×150 mm),volume ratio of methanol to water 85∶15 as the mobile phase,flow rate of the mobile phase 1.0 mL/min,UV absorption wavelength 220 nm,column temperature 27℃ and sample dosage 6 μL.The calibration curves of AMPS and AM were established.Their correlation coefficients were above 0.9995.The recoveries of the two components were in the range of 97.50％-100.62％ and the relative standard deviations were in the range of 0.435 7％-1.2981％.The method is accurate,rapid and sensitive.%建立了一种同时测定2-丙烯酰胺基-2-甲基丙磺酸(AMPS)/丙烯酰胺(AM)二元共聚物中残余单体AMPS和AM含量的HPLC法；为降低试样的黏性,以异丙醇-乙醇的混合液为提取剂,将AMPS和AM从AMPS/AM二元共聚物的水溶液中提取出来；同时考察了波长和流动相配比对AMPS和AM分离效果的影响,得到了最佳色谱分析条件.实验结果表明,适宜的色谱分析条件为:采用ZORBAXSB-C18(4.0mm×50mm)液相色谱柱,以体积比为85∶15的甲醇-水混合液为流动相,流动相流1.0mL/min,检测波长220nm,柱温27℃,进样量6μL;建立了AMPS/AM二元共聚物中残余单体AMPS和AM的标准工作曲线,二者的线性相关系数均大于0.9995,回收率为97.50％～100.62％,相对标准偏差为0.4357％～1.2981％.该方法具有操作简便、分析速度快、分离效果好、灵敏、准确高等优点,可满足测试要求.