W. Mohammed, T. Safaa, Abou El-Alamin Mm, Nahla Ns, El-Hashash Ma
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引用次数: 0
摘要
本文提出并验证了同步荧光光谱法(SF)在水中使用δ λ ( λ)=30 nm在272 nm处测量SF,用于测定存在其酸、碱和氧化降解产物的bimatoprost。Bimatoprost在2 M HCL, 2 M NaoH和30% H2O2的胁迫条件下进行。采用LC-MS对降解产物进行鉴定。假设了降解的途径。研究并优化了不同实验参数对药物荧光的影响。比马前列素的线性范围在25 ~ 250 ng/mL,检出限为0.005 ng/mL,定量限为0.018 ng/mL。根据ICH指南对该方法进行了验证。将该方法应用于该药物及其降解物的测定,验证了该方法的准确性。平均加样回收率为99.39±1.08。精密度(重复性和中间性)试验的RSD值分别为0.569和1.28。所建立的方法可有效地用于该药眼科配方的分析。与已有的方法进行了统计比较,结果表明该方法准确度高,精密度好。该方法是一种绿色分析化学方法;所使用的溶剂为水,因此该方法适用于所研究药物的常规分析,而不会对环境产生有害影响
Utility of Synchronous Spectrofluorimetric Method for Rapid Selective Determination of Bimatoprost: Stress Stability Study and Green Analytical Application
Stability indicating Synchronous spectrofluorimetric (SF) method has been proposed and validated for the determination of bimatoprost in presence of its acid, base, and oxidative degradation products by measuring SF at 272 nm using delta lamba (âλ)=30 nm in water. Bimatoprost was subjected to stress conditions of 2 M HCL, 2 M NaoH and 30% H2O2 . The identification of degradation products were done by LC-MS. The pathway of degradation was postulated. The effect of different experimental parameters on the fluorescence of the drug was studied and optimized. The range of linearity was over 25-250 ng/mL, the detection limit of 0.005 ng/ mL, and quantitation limit of 0.018 ng/ mL for bimatoprost. The developed method was validated according to ICH guidelines. The accuracy was checked by applying the proposed method for the determination of the drug and it’s degradant. The mean recoveries percentages were found to be 99.39 ± 1.08. RSD values for precision (repeatability and intermediate) testing was 0.569 and 1.28 respectively. The developed method was applied effectively for analysis of the drug in its ophthalmic formulation. The developed method was statistically compared with the reported method revealing high accuracy with good precision. The suggested method was found to be a green analytical chemistry method; the solvent used is water and hence that method can be suitable for routine analysis of the studied drug without effecting the environment harmfully