摘要
目的:建立一种不需杂质对照测定马来酸氟伏沙明片中杂质的测定方法。方法:通过马来酸氟伏沙明参与化学反应产生定位杂质,样品中杂质测定方法采用HPLC,色谱柱为Kromasil KR100-5C8(4.6mm×250 mm,5μm),以含1.25%磷酸氢二铵与0.275%庚烷磺酸钠的溶液(用磷酸调节pH至3.0)-甲醇(45∶55)为流动相,检测波长为254 nm。结果:马来酸氟伏沙明在碱加热条件下与马来酸合成反应,生成杂质Ⅲ。在1 mol·L-1盐酸溶液条件下降解生成杂质Ⅱ和Ⅳ;各杂质在色谱条件下分离度良好,杂质含量范围为0.6%~1.3%。结论:马来酸氟伏沙明经破坏及加成反应后,可用于杂质定位;可用高效液相色谱法测定马来酸氟伏沙明片中杂质的含量。
Objective:To develop a method for determination of the impurites in fluvoxamine maleate tablets without reference substances.Methods:The locating impurities were produced by chemical reaction with fluvoxamine maleate.And the determination of the impurities in samples were performed on a Kromasil KR100-5 C8 column(4.6 mm×250 mm,5μm)with the solution of 1.25%di-ammonium hydrogen phosphate and 0.275%sodium heptanesulfonate(adjusted to pH 3.0 with phosphoric acid)-methanol(45∶55)as mobile phase by HPLC.The detection wavelength was 254 nm.Results:ImpurityⅢwas synthetized by the fluvoxamine maleate reacted with maleic acid under the condition of alkali and heating.ImpurityⅡand impurityⅣwere produced by degradation under the condition of 1 mol·L-1 hydrochloric acid solution.All the impurities were separated well in chromatographic conditions,and the contents of the total impurities ranged from 0.6%to 1.3%.Conclusion:It can be used for locating impurities through destruction and addition reaction of fluvoxamine maleate.The contents of the impurities in fluvoxamine maleate tablets can be determined by HPLC.
作者
叶秀金
余少文
陈英
YE Xiu-jin;YU Shao-wen;CHEN Ying(Guangdong Institute for Drug Control,Guangzhou,510663,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2020年第9期1612-1618,共7页
Chinese Journal of Pharmaceutical Analysis
