C.B. Patel Research Centre, 3rd Floor, Bhaidas Hall, Vile Parle West, Mumbai 400056, India. sneha
J Pharm Biomed Anal. 2010 Jul 8;52(3):362-71. doi: 10.1016/j.jpba.2009.10.021. Epub 2009 Oct 31.
A simple, precise and stability-indicating HPLC method was developed and validated for the simultaneous determination of bisoprolol fumarate and hydrochlorothiazide in pharmaceutical dosage form. The method involves the use of easily available inexpensive laboratory reagents. The separation was achieved on an Inertsil ODS 3V (25cmx4.6mm) 5microm column with isocratic flow. The mobile phase at a flow rate of 1.0mLmin(-1), consisted of 0.1M potassium dihydrogen phosphate buffer and acetonitrile (70:30, v/v). The UV detection was carried out at 228nm. A linear response was observed over the concentration range 2.5-50microgmL(-1) of bisoprolol fumarate and the concentration range 6.25-125microgmL(-1) of hydrochlorothiazide. Limit of detection and limit of quantitation for bisoprolol fumarate were 0.01 and 0.03microgmL(-1), respectively and for hydrochlorothiazide were 0.01 and 0.05microgmL(-1), respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for specificity, linearity, accuracy, precision, robustness, ruggedness and system suitability. Individual drugs (bisoprolol fumarate and hydrochlorothiazide), their combinations and the tablets were exposed to thermal, photolytic, hydrolytic and oxidative stress conditions. The resultant stressed samples were analyzed by the proposed method. The method gave high resolution among the degradation products and the analytes. The peak purity of analyte peaks in the stressed samples was confirmed by photodiode array detector. The method was used for accelerated stability study on marketed and in-house formulations. The analysis concluded that the method was selective for simultaneous estimation of bisoprolol fumarate and hydrochlorothiazide and was stability-indicating.
建立并验证了一种用于同时测定药物制剂中富马酸比索洛尔和氢氯噻嗪的简单、精确且具有稳定性指示的 HPLC 方法。该方法使用易得且廉价的实验室试剂。分离是在 Inertsil ODS 3V（25cmx4.6mm）5μm 柱上进行的，采用等度洗脱。流动相为 0.1M 磷酸二氢钾缓冲液和乙腈（70:30，v/v），流速为 1.0mL/min。在 228nm 处进行紫外检测。富马酸比索洛尔的浓度范围为 2.5-50μg/mL 时呈线性响应，氢氯噻嗪的浓度范围为 6.25-125μg/mL 时呈线性响应。富马酸比索洛尔的检测限和定量限分别为 0.01 和 0.03μg/mL，氢氯噻嗪的检测限和定量限分别为 0.01 和 0.05μg/mL。该方法按照 ICH 指南的专属性、线性、准确性、精密度、稳健性、耐用性和系统适用性验收标准进行了成功验证。单独的药物（富马酸比索洛尔和氢氯噻嗪）、它们的组合和片剂都暴露于热、光解、水解和氧化应激条件下。用所提议的方法分析了产生的应激样品。该方法在降解产物和分析物之间给出了高分辨率。用光电二极管阵列检测器确认了应激样品中分析物峰的峰纯度。该方法用于市售和内部制剂的加速稳定性研究。分析表明，该方法对富马酸比索洛尔和氢氯噻嗪的同时估计具有选择性，并且具有稳定性指示作用。
