甲基丙烯酸-丙烯酸乙酯共聚物残留单体分析

Residual Monomer Analysis of Methacrylic Acid-Ethyl Acrylate Copolymer

目的:建立甲基丙烯酸-丙烯酸乙酯共聚物(物质的量比1∶1)中残留单体的测定方法。方法:采用高效液相色谱法。色谱柱为Agilent ZORBAX SB-C_(18)(4.6×150 mm,5μm),磷酸盐缓冲液(用磷酸溶液调节pH值至2.0)为流动相A,甲醇为流动相B,流速为1.0 mL/min,检测波长为202 nm,柱温为20℃。结果:甲基丙烯酸-丙烯酸乙酯共聚物(物质的量比1∶1)各主峰与相邻杂质峰分离度良好,甲基丙烯酸和丙烯酸乙酯在浓度0.1~2.0μg/mL范围内均与其峰面积呈现良好的线性关系(r^(2)=0.9999,0.9994);精密度和重复性的相对标准偏差(RSD)均小于2%;稳定性试验表明供试品溶液不稳定应临用现配;甲基丙烯酸和丙烯酸乙酯平均加标回收率分别为97.22%(RSD=4.12%),107.78%(RSD=1.93%)。结论:经方法学验证,此方法具有操作简单、快速灵敏、准确等优点,适用于甲基丙烯酸-丙烯酸乙酯共聚物(物质的量比1∶1)残留单体的测定。

Objetive:To establish a high-performance liquid chromatography(HPLC)method for the determination of residual monomers of methacrylic acid-ethyl acrylate copolymer(1∶1).Methods:The determination was carried out on a Agilent ZORBAX SB-C_(18)(4.6×150 mm,5μm)column,with phosphate buffer(by phosphoric acid solution adjust to pH 2.0)as mobile phase A and methanol as mobile phase B.The flow rate was 1.0 mL/min,the UV detection wavelength was set at 202 nm and the column temperature was 20℃.Results:The linear range was 0.1~2.0μg/mL for both methacrylic acid(r^(2)=0.9999)and ethyl acrylate(r^(2)=0.9994);The relative standard deviation of precision and repeatability were less than 2%.The experiments show that the test solution is unstable and should be prepared temporarily.The average recoveries of methacrylic acid and ethyl acrylate were 97.22%,107.78%with the relative standard deviation of 4.12%and 1.93%.Conclusion:The method is validated that it has the advantages of simple operation and accurate results.It can be used for the determination of residual monomers of methacrylic acid-ethyl acrylate copolymer(1∶1).