采用环糊精修饰的微乳液电动色谱法对硫酸右旋苯丙胺的杂质进行分析。
Impurity profiling of dexamphetamine sulfate by cyclodextrin-modified microemulsion electrokinetic chromatography.
机构信息
Department of Medicinal/Pharmaceutical Chemistry, Friedrich Schiller University Jena, Philosophenweg 14, Jena, Germany.
出版信息
Electrophoresis. 2010 Sep;31(17):3006-11. doi: 10.1002/elps.201000277.
A CD-modified microemulsion electrokinetic chromatography method has been developed and validated for dexamphetamine sulfate which allows the simultaneous determination of charged and uncharged impurities of the drug including the levorotary (R)-enantiomer. The optimized background electrolyte consisted of 1.5% w/w SDS, 0.5% w/w ethyl acetate, 3.5% w/w 1-butanol, 2.5% w/w 2-propanol and 92% w/w 50 mM sodium phosphate buffer, pH 3.0, containing 5.5% w/w sulfated β-CD. Separations were performed in a 50.2/40 cm, 50 μm id fused silica capillary at a temperature of 20°C and an applied voltage of -14 kV. Carbamazepine was used as internal standard. The assay was validated in the range of 0.1-1.0% for the related substances and 0.1-5.0% for levoamphetamine based on a concentration of 3 mg/mL of dexamphetamine sulfate. The LOD of all analytes ranged between 0.05 and 0.2%. In commercial samples of dexamphetamine sulfate, levoamphetamine was found at concentrations between 3.2 and 3.8%, whereas none of the other impurities could be detected.
已开发并验证了一种 CD 修饰的微乳液电动色谱法，用于硫酸右旋苯丙胺，该方法允许同时测定药物的带电和不带电杂质，包括左旋（R）对映异构体。优化的背景电解质由 1.5%w/w SDS、0.5%w/w 乙酸乙酯、3.5%w/w 1-丁醇、2.5%w/w 2-丙醇和 92%w/w 50 mM 磷酸钠缓冲液（pH 3.0）组成，其中含有 5.5%w/w 硫酸化β-CD。在 50.2/40cm、50μm id 的熔融石英毛细管中，于 20°C 温度和-14 kV 的施加电压下进行分离。卡马西平用作内标。基于 3mg/mL 硫酸右旋苯丙胺浓度，有关物质的测定范围为 0.1-1.0%，左旋苯丙胺的测定范围为 0.1-5.0%。所有分析物的 LOD 均在 0.05 至 0.2%之间。在硫酸右旋苯丙胺的商业样品中，发现左旋苯丙胺的浓度在 3.2 至 3.8%之间，而其他杂质均无法检测到。
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