The current work integrates design of experiment (DoE) techniques for developing, validating, and quantifying Cefotaxime sodium through RP-HPLC. Four independent factors were considered: flow rate, mobile phase ratio, oven temperature, and injection volume. A full factorial design was applied to optimize the parameters and determine the significant variables. Using the DoE approach, a more environmentally friendly separation and quantification were achieved with the help of the Venusil XBP. C8 column (5 um × 4.6 × 250 mm), a flow rate of 0.8 ml/minute, and a mobile phase ratio consisting of a binary combination of A:B (15:65). The organic phase (A) consisted of acetonitrile, while the aqueous phase (B) consisted of ammonium acetate, and the pH was adjusted to 6.1 with the aid of glacial acetic acid. The injection volume was set at 20 μl, and the elution was performed at a wavelength of 235 nm using a UV detector. The method was validated according to International Conference on Harmonisation guidelines, and it successfully determined the amount of Cefotaxime in Cefotaxime-loaded nanosponges. Tools such as Analytical Greenness metric (AGREE), “National Environmental Method Index” (NEMI), and “Green Analytical Procedure Index” (GAPI) were used to assess the greenness of the proposed method, along with a comparison of the proposed method with other reported HPLC methods. The proposed method proved to be eco-friendly, with better qualitative and quantitative results, as well as greener NEMI and GAPI quadrants. It also achieved a higher AGREE score (0.68) than the reported method (0.44).
Nair A, Chandrashekhar HR, Nayak UY. RP-HPLC method for quantification of cefotaxime sodium by using design of experiment, a green analytical approach: Analytical method development, validation, and application. J Appl Pharm Sci. 2024. Online First. http://doi.org/10.7324/JAPS.2024.192430
1. USP Monographs: Cefotaxime sodium [Internet]. [cited 2023 May 18]. Available from: http://www.pharmacopeia.cn/v29240/usp29nf24s0_m14080.html | |
2. Ling SSN, Yuen KH, Barker SA. Simple liquid chromatographic method for the determination of cefotaxime in human and rat plasma. J Chromatogr B. 2003 Jan 5;783(1):297-301. https://doi.org/10.1016/S1570-0232(02)00657-8 | |
3. . Rudnicki K, Sobczak K, Kaliszczak M, Sipa K, Powa?ka E, Skrzypek S, et al. Voltammetric study of cefotaxime at the macroscopic and miniaturized interface between two immiscible electrolyte solutions. Microchim Acta. 2021 Nov 9;188(12):413. https://doi.org/10.1007/s00604-021-05072-w | |
4. Melekhin AO, Tolmacheva VV, Goncharov NO, Apyari VV, Dmitrienko SG, Shubina EG, et al. Multi-class, multi-residue determination of 132 veterinary drugs in milk by magnetic solid-phase extraction based on magnetic hypercrosslinked polystyrene prior to their determination by high-performance liquid chromatography - tandem mass spectrometry. Food Chem. 2022 Sep 1;387:132866. https://doi.org/10.1016/j.foodchem.2022.132866 | |
5. Molecules | Free Full-Text | Green chemometric determination of cefotaxime sodium in the presence of its degradation impurities using different multivariate data processing tools; GAPI and AGREE Greenness Evaluation [Internet]. [cited 2024 Apr 27]. Available from: https://www.mdpi.com/1420-3049/28/5/2187 https://doi.org/10.3390/molecules28052187 | |
6. Nabi SA, Laiq E, Islam A. Selective separation and determination of cephalosporins by tlc on stannic oxide layers. Acta Chromatogr 14(14) 92-101. | |
7. Salem H, Samir E. Determination of cefotaxime, cefoperazone, ceftazidime and cefadroxil using surface plasmon resonance band of silver nanoparticles. Braz J Pharm Sci. 2018 Nov 29;54:e17565. https://doi.org/10.1590/s2175-97902018000317565 | |
8. Martínez-Piernas AB, Plaza-Bolaños P, Gilabert A, Agüera A. Application of a fast and sensitive method for the determination of contaminants of emerging concern in wastewater using a quick, easy, cheap, effective, rugged and safe-based extraction and liquid chromatography coupled to mass spectrometry. J Chromatogr A. 2021 Sep 13;1653:462396. https://doi.org/10.1016/j.chroma.2021.462396 | |
9. Kumar ACH, Gurupadayya BM, Sloka SN. Determination and validation of cefadroxil, ceftriaxone and cefotaxime by using n-bromosuccinamide in human plasma and pharmaceutical dosage form. Int J Res Pharm Sci. 2011 May 31;2(2):206-12. | |
10. Wang R, Jia ZP, Fan JJ, Jun M, Hua X, Zhang Q, et al. Separation and determination of cefotaxime enantiomers in injections by capillary zone electrophoresis. Die Pharmazie - Int J Pharm Sci. 2009 Mar 1;64(3):156-60. | |
11. Omar MA, Abdelmageed OH, Attia TZ. Kinetic spectrofluorimetric determination of certain cephalosporins in human plasma. Talanta. 2009 Feb 15;77(4):1394-404. https://doi.org/10.1016/j.talanta.2008.09.040 | |
12. Kelani KM, Elzanfaly ES, Saad AS, Halim MK, El-Zeiny MB. Different greenness assessment perspectives for stability-indicating RP-HPLC method used for the assay of isoxsuprine hydrochloride and four nephrotoxic and hepatotoxic photothermal degradation products. Microchem J. 2021 Dec 1;171:106826. https://doi.org/10.1016/j.microc.2021.106826 | |
13. El-Sayed HM, Hashem H. Quality by design strategy for simultaneous HPLC determination of bromhexine HCl and its metabolite ambroxol HCl in dosage forms and plasma. Chromatographia. 2020 Sep 1;83(9):1075-85. https://doi.org/10.1007/s10337-020-03924-w | |
14. Kannaiah KP, Sugumaran A. Environmental benign AQbD based estimation of ketoconazole and beclomethasone by RP-HPLC and multi-analytical UV spectrophotometric method. Microchem J. 2022;172:106968. https://doi.org/10.1016/j.microc.2021.106968 | |
15. Wadhwa G, Krishna KV, Dubey SK, Taliyan R. Development and validation of RP-HPLC method for quantification of repaglinide in mPEG-PCL polymeric nanoparticles: QbD-driven optimization, force degradation study, and assessment of in vitro release mathematic modeling. Microchem J. 2021 Sep 1;168:106491. https://doi.org/10.1016/j.microc.2021.106491 | |
16. Politis SN, Colombo P, Colombo G, Rekkas DM. Design of experiments (DoE) in pharmaceutical development. Drug Dev Ind Pharm. 2017;43(6):889-901. https://doi.org/10.1080/03639045.2017.1291672 | |
17. Anastas PT, Kirchhoff MM. Origins, current status, and future challenges of green chemistry. Acc Chem Res. 2002;35(9):686-94. https://doi.org/10.1021/ar010065m | |
18. Ga?uszka A, Migaszewski Z, Namie?nik J. The 12 principles of green analytical chemistry and the SIGNIFICANCE mnemonic of green analytical practices. Trends Anal Chem. 2013 Oct 1;50:78-84. https://doi.org/10.1016/j.trac.2013.04.010 | |
19. Nishio T, Kanazawa H. Green bioanalytical chemistry. In: Handbook of green analytical chemistry [Internet]. Hoboken, NJ: John Wiley & Sons, Ltd; 2012 [cited 2023 Jun 30]. pp. 425-47. Available from: https://onlinelibrary.wiley.com/doi/abs/10.1002/9781119940722.ch20 https://doi.org/10.1002/9781119940722.ch20 | |
20. Mohamed HM. Green, environment-friendly, analytical tools give insights in pharmaceuticals and cosmetics analysis. Trends Anal Chem. 2015 Mar 1;66:176-92. https://doi.org/10.1016/j.trac.2014.11.010 | |
21. El-Maraghy CM. Implementation of green chemistry to develop HPLC/UV and HPTLC methods for the quality control of fluconazole in presence of two official impurities in drug substance and pharmaceutical formulations. Sustain Chem Pharm. 2023 Jun 1;33:101124. https://doi.org/10.1016/j.scp.2023.101124 | |
22. Capello C, Fischer U, Hungerbühler K. What is a green solvent? a comprehensive framework for the environmental assessment of solventsof solvents. Green Chem. 2007 Aug 28;9(9):927-34. https://doi.org/10.1039/b617536h | |
23. Alfonsi K, Colberg J, Dunn PJ, Fevig T, Jennings S, Johnson TA, et al. Green chemistry tools to influence a medicinal chemistry and research chemistry based organisation. Green Chem. 2008 Jan 3;10(1):31-6. https://doi.org/10.1039/B711717E | |
24. Khurana RK, Rao S, Beg S, Katare OP, Singh B. Systematic development and validation of a thin-layer densitometric bioanalytical method for estimation of mangiferin employing analytical quality by design (AQbD) Approach. J Chromatogr Sci. 2016 May;54(5):829-41. https://doi.org/10.1093/chromsci/bmw001 | |
25. Palmer AC, Sorger PK. Combination cancer therapy can confer benefit via patient-to-patient variability without drug additivity or synergy. Cell. 2017 Dec 14;171(7):1678-91.e13. https://doi.org/10.1016/j.cell.2017.11.009 | |
26. Younis SE, El-Nahass SA, Soliman SA, Youssef RM. Simultaneous micro-determination of eplerenone and torsemide in their combined tablets using HPTLC-Dual wavelength spectrodensitometric and spectrophotometric methods. Microchem J. 2020 Jul;156:104861. https://doi.org/10.1016/j.microc.2020.104861 | |
27. Goto T, Yoshida Y, Kiso M, Nagashima H. Simultaneous analysis of individual catechins and caffeine in green tea. J Chromatogr. 1996 Oct 18;749(1):295-9. https://doi.org/10.1016/0021-9673(96)00456-6 | |
28. Mostafa F. Al-Hakkani. HPLC analytical method validation for determination of cefotaxime in the bulk and finished pharmaceutical dosage form. SCE. 2020 Mar 30;33-42. https://doi.org/10.37256/sce.112020199.33-42 | |
29. Asela I, Donoso-González O, Yutronic N, Sierpe R. β-Cyclodextrin-based nanosponges functionalized with drugs and gold nanoparticles. Pharmaceutics. 2021 Apr 8;13(4):513. https://doi.org/10.3390/pharmaceutics13040513 | |
30. Almutairy BK, Alshetaili A, Alali AS, Ahmed MM, Anwer MK, Aboudzadeh MA. Design of olmesartan medoxomil-loaded nanosponges for hypertension and lung cancer treatments. Polymers. 2021 Jan;13(14):2272. https://doi.org/10.3390/polym13142272 | |
31. P?otka J, Tobiszewski M, Sulej AM, Kupska M, Górecki T, Namie?nik J. Green chromatography. J Chromatogr. 2013 Sep;1307:1-20. https://doi.org/10.1016/j.chroma.2013.07.099 | |
32. Shah P, Patel J, Patel K, Gandhi T. Development and validation of an HPTLC method for the simultaneous estimation of Clonazepam and Paroxetine hydrochloride using a DOE approach. J Taibah Univ Sci. 2017 Jan 1;11(1):121-32. https://doi.org/10.1016/j.jtusci.2015.11.004 | |
33. Shabir G. Step-by-step analytical methods validation and protocol in the quality system compliance industry. J Valid Technol [Internet]. 2004 [cited 2023 Jun 30]. Available from: https://www.semanticscholar.org/paper/Step-by-step-analytical-methods-validation-and-in-Shabir/68718039ed36445c5e02c1100f21632f6858eff1 | |
34. Sharma T, Khurana RK, Jain A, Katare Op, Singh B. Development of a validated liquid chromatographic method for quantification of sorafenib tosylate in the presence of stress-induced degradation products and in biological matrix employing analytical quality by design approach. Biomed Chromatogr. 2018;32(5):e4169. https://doi.org/10.1002/bmc.4169 | |
35. Emergency Planning and Community Right-to-Know Act Section 313. Guidance for reporting toxic chemicals: polycyclic aromatic compounds category. | |
36. US EPA O. TRI-listed chemicals [Internet]. 2013 [cited 2023 May 21]. Available from: https://www.epa.gov/toxics-release-inventory-tri-program/tri-listed-chemicals | |
37. P?otka-Wasylka J. A new tool for the evaluation of the analytical procedure: green analytical procedure index. Talanta. 2018;181:204-9. https://doi.org/10.1016/j.talanta.2018.01.013 | |
38. Pena-Pereira F, Wojnowski W, Tobiszewski M. AGREE-Analytical GREEnness metric approach and software. Anal Chem. 2020;92(14):10076-82. https://doi.org/10.1021/acs.analchem.0c01887 | |
39. First report of columnea latent viroid (CLVd)in Gloxinia gymnostoma, G. nematanthodes and G. purpurascens in a botanical garden in Denmark-Nielsen-2010-New Disease Reports- Hoboken, NJ: Wiley Online Library [Internet]. [cited 2023 May 21]. Available from: https://bsppjournals.onlinelibrary.wiley.com/doi/10.5197/j.2044-0588.2010.022.004 | |
40. Garrigues S, de la Guardia M. Non-invasive analysis of solid samples. Trends Anal Chem. 2013 Feb 1;43:161-73. https://doi.org/10.1016/j.trac.2012.10.008 | |
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