聚丙烯酸树脂系列中残留单体的测定  

Determination of residual monomers in polyacrylic resin series

作　　者：卫星红 唐秀秀 张绍国 谢子立 WEI Xinghong;TANG Xiuxiu;ZHANG Shaoguo;XIE Zili(Anhui Institute for Food and Drug Control,Hefei 230051,China;Anhui University of Chinese Medicine,Hefei 230038,China;Lianyungang Wantai Pharmaceutical Materials Co.Ltd.,Lianyungang 222023,China)

机构地区：[1]安徽省食品药品检验研究院,合肥230051 [2]安徽中医药大学,合肥230038 [3]连云港万泰医药材料有限公司,江苏连云港222023

出　　处：《中国药品标准》2021年第3期208-215,共8页Drug Standards of China

基　　金：国家药典委员会标准制修订项目(2019Y003)。

摘　　要：目的:建立高效液相色谱法测定聚丙烯酸树脂系列中残留单体的方法。方法:采用高效液相色谱法,Phenomenex Luna C_(18)色谱柱(4.6 mm×150 mm, 5μm),流速为1.0 mL·min^(-1),柱温为35℃;聚丙烯酸树脂Ⅱ和聚丙烯酸树脂Ⅲ:流动相为甲醇-水(用磷酸调pH至2.0)(20∶80),检测波长为202 nm;聚丙烯酸树脂Ⅳ:流动相为磷酸盐缓冲液(pH 2.0)-甲醇(50:50),检测波长:205nm。结果:聚丙烯酸树脂Ⅱ和聚丙烯酸树脂Ⅲ中甲基丙烯酸、甲基丙烯酸甲酯分别在0.347~11.570μg·mL^(-1)(r=0.999 9,n=5)、0.334~11.120μg·mL^(-1)(r=0.999 6,n=5)浓度范围内与峰面积的线性关系良好,甲基丙烯酸平均回收率分别为99.5%(RSD=0.4%,n=9)和99.3%(RSD=0.4%,n=9),甲基丙烯酸甲酯平均回收率为99.2%(RSD=0.6%,n=9)和101.9%(RSD=2.0%,n=9)。聚丙烯酸树脂Ⅳ中甲基丙烯酸甲酯和甲基丙烯酸丁酯分别在2.026~202.6μg·mL^(-1)(r=0.999 8,n=5)、2.123~212.3μg·mL^(-1)(r=1.000 0,n=5)浓度范围内与峰面积的线性关系良好。甲基丙烯酸甲酯平均回收率为100.4%(RSD=1.1%,n=9),甲基丙烯酸丁酯平均回收率为97.7%(RSD=1.7%,n=9)。结论:建立的测定方法灵敏、准确,可用于聚丙烯酸树脂系列中单体的测定。Objective:To establish an HPLC method for the determination of residual monomers in polyacrylic resin series.Methods:HPLC was performed to determine residual monomers on Phenomenex Luna C 18 column(4.6 mm×150 mm,5μm)under conditions of column temperature of 35℃and flow rate of 1.0 mL·min^(-1).Polyacrylic resinⅡand polyacrylic resinⅢwas analyzed with a mobile phase of methanol-water(pH adjusted to 2.0 with phosphoric acid)(20∶80)at a wavelength of 202 nm.The analysis of polyacrylic resinⅣwas performed with a mobile phase of phosphate buffer solution(pH 2.0)-methanol(50∶50)at a wavelength of 205 nm.Results:The linear range of methacrylic acid in polyacrylic resinⅡand polyacrylic resinⅢfell into 0.347^(-1)1.570μg·mL^(-1)(r=0.9999,n=5)with corresponding recovery values of 99.5%(RSD=0.4%,n=9)and 99.3%(RSD=0.4%,n=9).The linear range of methyl methacrylate in polyacrylic resinⅡand polyacrylic resinⅢfell into 0.334^(-1)1.120μg·mL^(-1)(r=0.9996,n=5)with corresponding recovery values of 99.2%(RSD=0.6%,n=9)and 101.9%(RSD=2.0%,n=9).The linear ranges of methyl methacrylate and butyl methacrylate in polyacrylic resinⅣfell into 2.026-202.6μg·mL^(-1)(r=0.9998,n=5)with recovery of 100.4%(RSD=1.1%,n=9)and 2.123-212.3μg·mL^(-1)(r=1.0000,n=5)with recovery of 97.7%(RSD=1.7%,n=9),respectively.Conclusion:This method is sensitive,accurate and highly applicable for the determination of monomers in polyacrylic resin series.

关 键 词：聚丙烯酸树脂Ⅱ 聚丙烯酸树脂Ⅲ 聚丙烯酸树脂Ⅳ 甲基丙烯酸 甲基丙烯酸甲酯 甲基丙烯酸丁酯 HPLC 

分 类 号：R921.2[医药卫生—药学]