摘要
建立了高效液相色谱测定磺胺二甲嘧啶药物中4-氨基苯酚杂质的分析方法，严格按照美国药典USP29〈1225〉、人用药品注册技术国际协调会议指导文件ICH Q2A和ICH Q2B对方法进行了验证。色谱柱采用Phenomenex Luna C18（4．6×250mm，5μm）反相色谱柱，流动相为V（Na2HPO4（8．95g／L））：V（NaH2PO4（3．90g／L））：V（甲醇）=3：3：2，检测波长为235nm。当4-氨基苯酚的浓度在0．05～1．00μg／mL时，色谱峰面积与浓度呈良好的线性关系，线性相关系数R=0．9993。方法的检出限为2．0mg／kg，定量限为5．0mg／kg。方法的准确度、精密度和专属性均满足USP29〈1225〉、ICHQ2A和ICHQ2B的要求。将方法用于实际磺胺二甲嘧啶原料药检测，结果未检出含有4-氨基苯酚。本方法适合于磺胺二甲嘧啶及类似药物中4-氨基苯酚杂质的检测。
A method for the determination of 4-aminophenol impurities in sulfadimidine drug by high performance liquid chromatography （HPLC） was developed and validated strictly following USP29 〈 1225 〉 , ICH Q2A and ICH Q2B. The analysis was performed on a Phenomenex reversed phase Luna column ClS （4.6 × 250 mm, 5 μm）. A mo- bile phase of Na2 HPO4 （ 8.95 g/L） ： NaH2PO4 （3.90 g/L） ： Methanol = 3 ： 3 ： 2 and a UV wavelength of 235 nm were used for separation and determination of 4-aminophenol. The linear range was from 0.05 to 1.00/_tg/mL and linear correlation coefficient was 0.9993. The limit of detection （LOD） and limited of quantitation （LOQ） were 2.0 and 5.0 mg/kg, respectively. The accuracy, precision and specificity of the method have met the requirement of USP29 〈 1225 〉 , ICH Q2A and ICH Q2B. The method was also used to detect sulfadimidine drug samples, and none of the 4-aminophenol was detected in samples. The method was simple, fast, sensitive, accurate, and suitable to detect 4-aminophenol impurities in sulfadimidine and similar drag products, quality control and supervision.
出处
《分析试验室》
CAS
CSCD
北大核心
2009年第6期108-111,共4页
Chinese Journal of Analysis Laboratory
