Ragab Gamal H, Saleh Hanaa M, Abdulla Nermeen M, Bahgat Eman A
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Zagazig University, Zagazig, 44519, Egypt.
BMC Chem. 2023 Aug 5;17(1):94. doi: 10.1186/s13065-023-01006-0.
In a new attempt to separate some sulbactam combinations by green chemical method we came up with this research in which an ecofriendly, green, sustainable and selective method was established for separation of four antibiotics, namely, cefoperazone (CFP), cefixime (CFX), ampicillin (AMP) and sulbactam (SLB). No organic solvents were used in the composition of the mobile phase as it was replaced by mixing two surfactants together, sodium dodecyl sulfate (SDS) and polyoxyethylene-23-lauryl ether (Brij-35). Effect of varying the concentrations of the two surfactants on chromatographic separation was studied. Optimum separation was maintained using a mobile phase consisting of 0.01 mol/L SDS, 0.03 mol/L Brij-35, 0.4% Tri-ethylamine (TEA) and pH of 2.8 adjusted by using 1 M ortho-phosphoric acid on reversed phase Isère C BDS column with temperature of 40 °C at flow rate 1 mL/min, wavelength 215 nm, and the total run time was 6 min. Validation of the proposed method has been made according International Conference of Harmonization (ICH) guidelines at linearity range of 10-200 µg mL for all drugs under study, high accuracy results (recovery range 98.39-100.35%). and the variation coefficient (RSD) of the points on the calibration curve was ranged from (0.1-1.7%) indicating precise method. The LOQ was (6.09 μg mL) for CFP, (6.07 μg mL) for CFX, (3.85 μg mL) for AMP and (7.20 μg mL) for SLB. Successful applications were made on marketed dosage forms with recovery range of (100.16-102.25%) and RSD of (0.03-1.88%). The method was verified on the Green Analytical Procedure Index (GAPI) and Analytical Greenness metric approach (AGREE) and it was found to be an excellent green alternative method.
在通过绿色化学方法分离某些舒巴坦组合的新尝试中，我们开展了这项研究，建立了一种生态友好、绿色、可持续且具有选择性的方法来分离四种抗生素，即头孢哌酮（CFP）、头孢克肟（CFX）、氨苄西林（AMP）和舒巴坦（SLB）。流动相的组成中未使用有机溶剂，而是通过将两种表面活性剂，十二烷基硫酸钠（SDS）和聚氧乙烯 - 23 - 月桂醚（Brij - 35）混合来替代。研究了改变两种表面活性剂浓度对色谱分离的影响。使用由0.01 mol/L SDS、0.03 mol/L Brij - 35、0.4%三乙胺（TEA）组成且pH值用1 M正磷酸调节至2.8的流动相，在反相Isère C BDS柱上，温度为40°C，流速为1 mL/min，波长为215 nm的条件下进行分离，总运行时间为6分钟，可实现最佳分离效果。根据国际协调会议（ICH）指南对所提出的方法进行了验证，所有研究药物的线性范围为10 - 200 μg/mL，结果具有高精度（回收率范围为98.39 - 100.35%），校准曲线上各点的变异系数（RSD）范围为（0.1 - 1.7%），表明该方法精确。CFP的定量限为（6.09 μg/mL），CFX为（6.07 μg/mL），AMP为（3.85 μg/mL），SLB为（7.20 μg/mL）。该方法成功应用于市售剂型，回收率范围为（100.16 - 102.25%），RSD为（0.03 - 1.88%）。该方法通过绿色分析程序指数（GAPI）和分析绿色度度量方法（AGREE）进行了验证，并被发现是一种优秀的绿色替代方法。
