摘要
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10μL,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IonPacAS11-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10μL,带DIONEX AERS500 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。
New methods were developed for the determination of succinic acid in desvenlafaxine succinate（DVS）by high performance ion-exclusion chromatography（HPIEC）and high performance ion-exchange chromatography（HPIC）. HPIEC and HPIC methods were used separately to determinate the succinic acid in DVS. With HPIEC,the sample was diluted with 2. 50×10-3mol / L sulfuric acid solution and filtrated by 0. 22 μm polyether sulfone filter membrane,and then analyzed by HPIEC directly without any further pretreatment. The analytical column was Phenomenex Rezex ROA-organic Acid H＋（8%）（300 mm×7. 8 mm）. The mobile phase was2. 50×10-3mol / L sulfuric acid solution at the flow rate of 0. 5 mL / min. The column temperature was set at 40 ℃,and the detection wavelength was 210 nm. The injection volume was 10 μL.The assay was quantified by external standard method. With HPIC,the sample was diluted with ultrapure water and filtrated by 0. 22 μm polyether sulfone filter membrane,and then analyzed by HPIC directly without any further pretreatment. The analytical column was Dionex IonPac AS11-HC（250 mm × 4 mm）with a guard column IonPacAG11-HC（50 mm × 4 mm）. Isocratic KOH elute generator was used at the flow rate of 1. 0 mL / min. The detection was performed by a Dionex suppressed（DIONEX AERS 500 4-mm）conductivity detector. The injection volume was 10 μL. The content computation was performed with peak area external reference method.The results of HPIEC method for succinic acid were 28. 8%,28. 9% and 28. 9%,while the results of HPIEC method were 28. 2%,28. 6% and 28. 6%. The results of HPIEC and HPIC methods were not significantly different. The two methods can both be used to determine the contents of succinic acid in DVS. The surveillance analytical method should be chosen according to the situation.
出处
《色谱》
CAS
CSCD
北大核心
2016年第2期189-193,共5页
Chinese Journal of Chromatography
基金
科技部新药创制重大专项平台项目(2012ZX09301002-001-019)
辽宁医学院横向课题(LYHX2013001)~~
关键词
高效离子抑制色谱法
高效离子交换色谱法
琥珀酸
琥珀酸去甲文拉法辛
high performance ion-exclusion chromatography（HPIEC）
high performance ionexchange chromatography
succinic acid
desvenlafaxine succinate（DVS）
