KU Leuven, Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, Herestraat 49, O&N2, PB, 923, Leuven 3000, Belgium; Wollo University, College of Medicine and Health Sciences, Department of Pharmacy P.O. Box 1145, Dessie, , Ethiopia.
KU Leuven, Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, Herestraat 49, O&N2, PB, 923, Leuven 3000, Belgium.
J Pharm Biomed Anal. 2024 Jul 15;244:116127. doi: 10.1016/j.jpba.2024.116127. Epub 2024 Mar 27.
Antimicrobials, particularly antibiotics, are among the most common classes of drugs reported as substandard and falsified (SF) in developing countries. Therefore, it is important to develop simple and affordable analytical methods for the quality control of antimicrobial medicines. In this study, a liquid chromatographic method with ultraviolet detection (LC-UV) was developed and validated for the screening and quantification of 13 antimicrobial medicines and one beta-lactamase inhibitor in pharmaceutical formulations. LC separation was carried out on a Kinetex C18 column (150 mm × 4.6 mm, 2.6 µm) with gradient elution. The mobile phase consisted of mixtures of acetonitrile-water-10 mM phosphate buffer pH 3.5 at ratios of 3:92:5, v/v/v for mobile phase A and 50:45:5, v/v/v for mobile phase B with a flow rate of 0.5 mL/min. The screening method was intended for confirmation of the identity of the actives and validated for specificity and robustness, whereas the quantification method (using only a different detection wavelength) was further validated in terms of linearity, accuracy, sensitivity and precision (repeatability, intermediate precision). For all compounds, the method was found to be linear (r > 0.999), precise (%RSD < 1%), accurate (% recovery of 98-102%), sensitive, specific and robust. The developed LC method was successfully applied for the identification and assay of 12 antimicrobial samples from Ethiopia. Among the 12 samples analyzed, one (8.3%) product was confirmed to be falsified.
抗菌药物，特别是抗生素，是发展中国家报告的不符合标准和假冒伪劣（SF）的最常见药物类别之一。因此，开发用于控制抗菌药物质量的简单且负担得起的分析方法非常重要。在这项研究中，开发并验证了一种用于药物制剂中 13 种抗菌药物和一种β-内酰胺酶抑制剂的筛选和定量的液相色谱法与紫外检测（LC-UV）。LC 分离在 Kinetex C18 柱（150mm×4.6mm，2.6μm）上进行，采用梯度洗脱。流动相由乙腈-水-10mM 磷酸盐缓冲液 pH 3.5 的混合物组成，比例为 3:92:5，v/v/v 用于流动相 A 和 50:45:5，v/v/v 用于流动相 B，流速为 0.5mL/min。筛选方法旨在确认活性成分的身份，并验证其特异性和稳健性，而定量方法（仅使用不同的检测波长）则进一步验证了线性、准确性、灵敏度和精密度（重复性、中间精密度）。对于所有化合物，该方法均表现出良好的线性（r＞0.999）、精密度（%RSD＜1%）、准确性（%回收率为 98-102%）、灵敏度、特异性和稳健性。所开发的 LC 方法成功地应用于来自埃塞俄比亚的 12 种抗菌药物样品的鉴定和测定。在所分析的 12 个样品中，有一个（8.3%）产品被确认为假冒伪劣。
