Ibesh Sherwan, Bitar Yaser, Trefi Saleh
Department of Pharmaceutical Chemistry and Quality Control, Faculty of Pharmacy, University of Aleppo, Aleppo, Syria.
Heliyon. 2023 Mar 3;9(3):e14189. doi: 10.1016/j.heliyon.2023.e14189. eCollection 2023 Mar.
A simple, precise, rapid, and eco-friendly FTIR spectrophotometric method was developed and validated for simultaneous analysis of amlodipine (AML) and atorvastatin (ATV) in drug combination preparations. Firstly, synthetic mixtures were made and scanned with FTIR instrument. Then the result spectra were converted automatically to absorbance spectra. The calibration model was made depending on Beer's law which relates concentration to absorbance. Two characteristic bands corresponding to the carbonyl group at 1708-1688 cm and 1660-1632 cm for AML and ATV, respectively, were selected for quantification. The absorbance of a series of standards was measured as the AUC of the chosen bands. Then, the calibration line was obtained by plotting the measured AUCs and the actual concentrations against each other. Validation tests were performed per ICH recommendations. Specificity was evaluated by the separation of APIs and excipients from marketed preparations by methanol. Then, the spectra of extracted excipients, APIs, and pharmaceutical samples were taken and overlapped. The selected peaks were specific and did not interfere with each other or other peaks from the excipients used in the tablet's matrix. Linearity for AML and ATV was in the range of 0.1-1% w/w with excellent coefficients of determination (R), 0.998 and 0.999 for AML and ATV, respectively. The proposed analytical method was accurate and precious, as the RSD values were less than 2%. The proposed FTIR method was successfully applied to estimate the exact quantity of APIs in pharmaceutical samples. Recoveries were accepted in accordance with USP and were in the range of 94.62-100.6% and 98.175-101.06% for AML and ATV, respectively. Likewise, the acquired results were compared with the HPLC method. And the t- and F- tests were calculated and compared with the theoretical values, which indicate the similarity of results in both developed and reported methods.
开发并验证了一种简单、精确、快速且环保的傅里叶变换红外光谱法，用于同时分析复方制剂中的氨氯地平（AML）和阿托伐他汀（ATV）。首先，制备合成混合物并用傅里叶变换红外光谱仪进行扫描。然后，将所得光谱自动转换为吸光度光谱。根据将浓度与吸光度相关联的比尔定律建立校准模型。分别选择AML和ATV在1708 - 1688 cm和1660 - 1632 cm处对应羰基的两个特征峰进行定量。测量一系列标准品的吸光度作为所选峰的曲线下面积（AUC）。然后，通过将测量的AUC与实际浓度相互绘制得到校准曲线。按照国际人用药品注册技术协调会（ICH）的建议进行验证试验。通过用甲醇从市售制剂中分离活性成分和辅料来评估特异性。然后，获取提取的辅料、活性成分和药物样品的光谱并进行叠加。所选峰具有特异性，彼此之间以及与片剂基质中使用的辅料的其他峰均不相互干扰。AML和ATV的线性范围为0.1 - 1% w/w，测定系数（R）分别为0.998和0.999，效果良好。所提出的分析方法准确且精密，相对标准偏差（RSD）值小于2%。所提出的傅里叶变换红外光谱法成功应用于估算药物样品中活性成分的准确含量。回收率符合美国药典要求，AML和ATV的回收率分别在94.62 - 100.6%和98.175 - 101.06%范围内。同样，将所得结果与高效液相色谱法进行比较。计算t检验和F检验并与理论值进行比较，结果表明所开发方法与已报道方法的结果相似。
