UPLC-MS/MS and Dushman reaction based spectrophotometric method for determination of Ceftazidime, an antibiotic, in medicinal formulation

ABSTRACT: Two analytical methods were developed, one utilizing sensitive UPLC-MS/MS method while other being the spectrophotometric method exploiting the Dushman reaction. Both methods were validated based on ICH guidelines and were successfully applied to quantitate the drug in marketed formulation. UPLC-MS/MS method responded linearly in the range of 1.6 µgmL-1-6.4 µgmL-1 while spectrophotometric procedure followed the Beer’s law in the concentration range of 30-100 µgmL-1. UPLC-MS/MS has been found to have a limit of quantitation of 0.97 µgmL-1 while spectrophotometric method was found to quantitate 14.00 µgmL-1 correctly with high precision. Both the methods showed an excellent recovery of 99.36%-100.91% (% RSD 1.05-1.73) and 98.64%-99.73% (%RSD 0.67-1.68) for UPLC-MS/MS and spectrophotometric, respectively.

摘要：本研究开发了两种分析方法：其一为灵敏度优异的超高效液相色谱-串联质谱（UPLC-MS/MS）法，另一则为利用杜什曼（Dushman）反应的分光光度法。两种方法均依据人用药品注册技术要求国际协调会（ICH）指南进行方法学验证，并成功应用于市售制剂中药物的含量测定。UPLC-MS/MS法的线性范围为1.6 μg·mL⁻¹至6.4 μg·mL⁻¹；分光光度法遵循比尔（Beer）定律，其线性浓度范围为30~100 μg·mL⁻¹。经测定，UPLC-MS/MS法的定量限为0.97 μg·mL⁻¹；分光光度法则可准确测定14.00 μg·mL⁻¹浓度的样品，且具有较高的精密度。两种方法的回收率均表现优异：UPLC-MS/MS法的回收率为99.36%~100.91%（相对标准偏差%RSD为1.05~1.73），分光光度法的回收率为98.64%~99.73%（%RSD为0.67~1.68）。