Moumita Saha, Ashutosh Gupta, Shiran Shetty, Srinivas Mutalik, K. Nandakumar, H. Raghu Chandrashekar, Namdev Dhas, Sudheer Moorkoth
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The multivariate Box–Behnken design (BBD) was utilized to optimize chromatographic parameters. Independent variable such as ratio of mobile phase, flow rate, pH and injections volume were optimized using DoE, and analyzed using perturbation plots. A desirability of 0.981 was achieved for the optimized variables. The optimized method utilized methanol and phosphate buffer (25:75) at pH 6.3 as the mobile phase in an isocratic elution mode on a Luna ODS C18 column kept at 25 °C as the stationary phase. The method was linear from 0.25 to 20 µg/mL, for both the drugs with R<sup>2</sup> values of 0.9993 and 0.9997 for amoxicillin and tinidazole, respectively. This validated RP-HPLC technique demonstrated selectivity in the presence of possible degradation products and excipients present in the mucoadhesive GRDDS beads. 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引用次数: 0
摘要
幽门螺杆菌（H. pylori）感染是全球消化性溃疡病的主要风险因素之一。由于抗生素无法有效进入幽门螺杆菌栖息的胃黏膜内层，因此使用传统剂型治疗幽门螺杆菌往往具有挑战性。本研究开发了一种环保、稳定的 RP-HPLC 方法，用于同时估算针对幽门螺杆菌感染的粘胶剂型中阿莫西林和替硝唑的含量。抗生素粘液黏附型GRDDS制剂的开发旨在提高胃黏膜的生物利用度。该研究采用多元盒-贝肯设计（BBD）来优化色谱参数。使用 DoE 对流动相比例、流速、pH 值和进样量等自变量进行了优化，并使用扰动图进行了分析。优化变量的可取性达到 0.981。优化后的方法以甲醇和 pH 值为 6.3 的磷酸盐缓冲液（25:75）为流动相，采用等度洗脱模式，以 25 °C 下的 Luna ODS C18 色谱柱为固定相。阿莫西林和替硝唑的R2值分别为0.9993和0.9997。这种经过验证的 RP-HPLC 技术在粘液黏附性 GRDDS 珠中可能存在降解产物和辅料的情况下也具有选择性。该方法被用于测定黏附性GRDDS制剂中替硝唑和阿莫西林的包埋效率和体外释放曲线。
DoE-Aided Optimization of RP-HPLC Method for Simultaneous Estimation of Amoxicillin and Tinidazole Loaded Mucoadhesive GRDDS Formulation for the Treatment of H. pylori
Helicobacter pylori (H. pylori) infection is one of the primary risk factors of peptic ulcer disease worldwide. Treatment of H. pylori with the conventional dosage form is often challenging due to the ineffective reach of the antibiotics to the inner layers of gastric mucosa, where the organism resides. This study developed an eco-friendly, stability-indicating RP-HPLC method to simultaneously estimate amoxicillin and tinidazole from mucoadhesive formulation targeting H. pylori infection. The mucoadhesive GRDDS formulation of antibiotics was developed with a goal of improving bioavailability at the gastric mucosa. The multivariate Box–Behnken design (BBD) was utilized to optimize chromatographic parameters. Independent variable such as ratio of mobile phase, flow rate, pH and injections volume were optimized using DoE, and analyzed using perturbation plots. A desirability of 0.981 was achieved for the optimized variables. The optimized method utilized methanol and phosphate buffer (25:75) at pH 6.3 as the mobile phase in an isocratic elution mode on a Luna ODS C18 column kept at 25 °C as the stationary phase. The method was linear from 0.25 to 20 µg/mL, for both the drugs with R2 values of 0.9993 and 0.9997 for amoxicillin and tinidazole, respectively. This validated RP-HPLC technique demonstrated selectivity in the presence of possible degradation products and excipients present in the mucoadhesive GRDDS beads. The method was used for the determination of entrapment efficiency and in vitro release profile for tinidazole and amoxicillin in the mucoadhesive GRDDS formulation.
期刊介绍：
Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.
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