Ultraviolet spectrophotometric method for analytical determination of mianserin hydrochloride in coated tablets and comparison with LC

abstract Ultraviolet spectrophotometric (UV) and Liquid Chromatographic (LC) methods for the determination of mianserin hydrochloride in pharmaceutical formulation were developed and validated. The various parameters, such as specificity, linearity, precision and accuracy were studied according to International Conference on Harmonization (ICH, 2005). For UV method, mianserin hydrochloride was determinate at 278 nm using HCl 0.1 M as the solvent. The response was linear in the concentration range of 20.0 - 140.0 µg/mL (r = 0.9998). Precision data evaluated by relative standard deviation was lower than 2%. The UV method was simple, rapid and low cost. Chromatographic analyses were performed in an Ace C18 column and the mobile phase was composed of methanol, 50 mM monobasic potassium phosphate buffer and 0.3% triethylamine solution adjusted to pH 7.0 with phosphoric acid 10% (85:15). LC method was specific, linear, precise, exact and robust. The results confirmed that the both methods are valid and useful to the routine quality control of mianserin hydrochloride in coated tablets. Statistical analysis by Student´s t-test showed no significant difference between the results obtained by UV and LC methods.摘要：本研究建立并验证了两种可用于药物制剂中盐酸米安色林含量测定的分析方法，分别为紫外分光光度法（Ultraviolet spectrophotometric，UV）与液相色谱法（Liquid Chromatographic，LC）。依据人用药品注册技术要求国际协调会（International Conference on Harmonization，ICH）2005年发布的指导原则，对方法的专属性、线性、精密度与准确度等关键验证参数进行了系统考察。 针对紫外分光光度法，以0.1 mol/L盐酸作为溶剂，在278 nm波长处对盐酸米安色林进行含量测定；该方法在20.0~140.0 μg/mL的浓度范围内响应值与浓度呈良好线性关系，相关系数r=0.9998。以相对标准偏差评估的精密度数据均低于2%，且具备操作简便、快速及成本低廉的优势。 液相色谱法采用Ace C18色谱柱进行分离，流动相由甲醇、50 mmol/L磷酸二氢钾缓冲液与0.3%三乙胺溶液按体积比85:15混合而成，并用10%磷酸溶液调节至pH 7.0。该液相色谱法具备专属性、线性、精密度、准确度与耐用性。 实验结果证实，两种方法均具备方法学可行性，可用于盐酸米安色林包衣片的日常质量控制。采用t检验（Student´s t-test）进行的统计学分析显示，紫外分光光度法与液相色谱法所得测定结果无显著性差异。