高效离子抑制色谱法和高效离子交换色谱法检测琥珀酸去甲文拉法辛中琥珀酸的含量

建立了用于琥珀酸去甲文拉法辛中琥珀酸含量测定的高效离子抑制色谱和高效离子交换色谱方法。离子抑制色谱法采用Rezex ROA-organic Acid H+(8%)色谱柱,以2.50×10^-3mol/L硫酸溶液为流动相等度洗脱,流速为0.5 mL/min,进样10 μ L,检测波长为210 nm,琥珀酸的含量按峰面积外标法计算;离子交换色谱法采用IonPac^® AS11-HC色谱柱,以氢氧化钾为淋洗液等度洗脱,流速为1.0 mL/min,进样10 μ L,带DIONEX AERS^® 500 4-mm抑制器的电导检测器检测,琥珀酸含量按峰面积外标法计算。两种方法对3批琥珀酸去甲文拉法辛中琥珀酸质量分数的测定结果分别为:28.8%、28.9%、28.9%和28.2%、28.6%、28.6%。离子抑制色谱法和离子交换色谱法在琥珀酸去甲文拉法辛中琥珀酸的含量测定结果上没有明显不同,可根据实际情况选择。     

Ionic organic/inorganic materials. III. Stimuli responsive hybrid hydrogels based on oligo(N,N‐dimethylaminoethylmethacrylate) and chloroalkyl‐functionalized siloxanes

Ionic organic/siloxane networks containing quaternary ammonium salt (QAS) sequences in the cross‐linking bridges were obtained by the Menshutkin reaction of oligo(N,N‐dimethylaminoethylmethacrylate) (ODMAEM) with a telechelic chloroalkylated siloxane (CAS), such as 1,3‐bis‐(chloromethyl)‐1,1,3,3‐tetramethyldisiloxane, 1,3‐bis‐(chloropropyl)‐1,1,3,3‐tetramethyldisiloxane, and α,ω‐bis(chloromethyl) oligodimethylsiloxane. The resulted structures were investigated by Fourier transform infrared spectroscopy emphasizing the presence of both organic and siloxane moieties. The thermogravimetric analysis under inert atmosphere of the networks, besides the thermal stability, gave also information on the composition of hybrid hydrogels. The morphology of the lyophilized networks was evidenced by environmental scanning electron microscopy, as a function of CAS structure and CAS: ODMAEM feed molar ratio. The swelling response of the ionic networks in water as a function of pH and counterion nature and concentration as well as the water vapors sorption capacity in dynamic regime were evaluated. The properties of the ionic hybrid hydrogels were correlated with the reactants feed molar ratio and concentration of the reaction mixture, CAS type, and the presence of a catalyst. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2009