摘要
以含0.01 mol·L^(-1)三氟乙酸钠的六氟异丙醇(HFIP)溶液(流动相)为溶剂溶解聚对二氧环己酮(PPDO)样品,使其质量浓度达到4 g·L^(-1)。过0.45μm滤膜,在凝胶色谱仪的Shodex HFIP 805/Shodex HFIP 803串联色谱柱上分离。多角度激光光散射仪的角度经聚甲基丙烯酸甲酯(PMMA)标准溶液进行归一化校正后,用来分析色谱仪分离得到的目标物,并将示差折光仪测得的折光指数增量代入光散射法测定绝对分子量的公式,计算PPDO的重均分子量、数均分子量及分子量分布指数。结果显示,重均分子量、数均分子量及分子量分布指数的相对标准偏差(n=6)均小于5.0%;PPDO在HFIP中的分子构象为无规线团状;凝胶色谱法所得重均分子量、数均分子量和分子量分布指数远大于上述方法的,主要由PMMA(用于制作标准曲线)和PPDO分子结构差异较大所致。
Hexafluoroisopropanol(HFIP) solution(mobile phase) containing 0.01 mol·L^(-1) sodium trifluoroacetate was used as the solvent to dissolve the sample of p-dioxycyclohexanone(PPDO), to make the mass concentration of the sample reach to 4 g·L^(-1). The sample solution was filtered with 0.45 μm filter membrane, and the separation was performed on the Shodex HFIP 805/Shodex HFIP 803 tandem columns of the gel chromatograph. The angle of the multi-angle laser light scatterer was normalized by the standard solution of polymethyl methacrylate(PMMA), and the detection was carried out on the target separated by the chromatograph. The increment of the refractive index measured by the differential refractometer was substituted into the formula for determining the absolute molecular weight by the light scattering method to calculate the weight-average molecular weight, number-average molecular weight and molecular weight distribution index of PPDO. As shown by the results that RSDs(n=6) of weight-average molecular weight, number-average molecular weight and molecular weight distribution index were all less than 5.0%. The molecular conformation of PPDO in HFIP was random line cluster. The weight-average molecular weight, number-average molecular weight and molecular weight distribution index obtained by gel chromatography were much higher than those obtained by the above method, mainly due to the large difference between molecular structures of PMMA(used for making the standard cure) and PPDO.
作者
彭健
施燕平
刘叶
沈永
刘莉莉
陈方
PENG Jian;SHI Yanping;LIU Ye;SHEN Yong;LIU Lili;CHEN Fang(Shandong Institute of Medical Device and Phar maceutical Packaging Inspection,Jinan 250101,China;NMPA Key Laboratory for Safety Evaluation of Biomaterials and Medical Devices,Jinan 250101,China;Shandong Key Laboratory of Biological Evaluation for Medical Devices,Jinan 250101,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2022年第11期1283-1286,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家重点研发计划项目(2016YFC1103205)
山东省医疗器械和药品包装检验研究院课题(ZX202009)。
关键词
凝胶色谱法
多角度激光光散射法
绝对分子量
分子量分布指数
聚对二氧环己酮
gel chromatography
multi-angle laser light scattering
absolute molecular weight
molecular weight distribution index
poly p-dioxycyclohexanone
