高效液相色谱法和非水电位滴定法测定注射用盐酸赖氨酸含量的比较

目的 分别建立高效液相色谱法和非水电位滴定法,用于测定注射用盐酸赖氨酸含量.方法 高效液相色谱法采用色谱柱为Phenomenex C18柱(250mm×4.6mm,5μm),流动相为甲醇-0.05 mol/L醋酸钠和醋酸溶液(60:40),流速1.0mL/min,检测波长为360nm,柱温为40 ℃;非水电位滴定法以醋酸汞和冰醋酸为溶剂,用0.1 mol/L高氯酸溶液进行滴定.结果 采用高效液相色谱法时,盐酸赖氨酸质量浓度在2.0～10.0μg/mL范围内与峰面积线性关系良好,r=0.999 5,方法精密度RSD为0.41%(n=6),平均回收率为98.8%,RSD为0.62%(n=9);采用非水电位滴定法时,方法精密度RSD为0.33%(n=6),平均回收率为99.6%,RSD为0.37%(n=9).结论 所采用的两种方法的测定结果无显著差异.高效液相色谱法分离能力高,专属性强,消耗样品量少,但该柱前衍生化高效液相色谱法操作繁杂,衍生化反应所需试剂难得;非水电位滴定法测定其电位突跃明显、易辨,操作简单、快速,测定结果精密,准确度高,成本低,能够满足其质量控制,更适合于常规检测,故采用非水电位滴定法测定该品含量,并订入其质量标准中.

Content Determination of Lysine Hydrochloride for Injection by HPLC and Non-Aqueous Potentiometry Titration

Objective To establish an HPLC method and a non-aqueous potentiometry titration method for the content determination of Lysine Hydrochloride for Injection.Methods The HPLC method was used.The separation was performed on the Phenomenex C18 column（250 mm×4.6 mm,5 μm）.The mobile phase was methanol-0.05 mol/L sodium acetate and acetic acid solution（60：40） at the flow rate of 1.0 mL/min.The UV detection was set at 360 nm and the column temperature was maintained at 40 ℃.Acetic acid and mercury acetate were used as solvent for the non-aqueous potentiomerry titration.0.1 mol/L perchloric acid was used to titrate the content of lysine hydrochloride.Results HPLC was adopted,the linear range for lysine hydrochloride was 2.0-10.0 μg/mL（r=0.999 5）,the precision RSD was 0.41%（n=6）;the average recovery rate was 98.8%with RSD 0.62%（n=9）.Non-aqueous potentiometry titration：the precision RSD was 0.33%（n=6）,the average recovery rate was 99.6%with RSD 0.37%（n=9）.Conclusion The HPLC method and non-aqueous potentimetry titration method have no significantly statistical difference.The HPLC method has the high separating ability and the strong specificity with small amount of sample consumption,however its pre-column derivatization is complicated and the required derivatization reagents are rare.The non-aqueous potentiometry titration method has clear potential-jump and is easy to distinguish and simply operate,rapid,with precise detection results,high accuracy and low cost,can meet its quality control,and is more suitable for routine testing.So the non-aqueous potentiometry titration method is adopted for the content determination of Lysine Hydrochloride for Injection,and set into its quality standards.