Skip to main content
Log in

Method Development for Determination of Antibiotic Drugs Using Newly Prepared p-Morpholinomethylcalix[4]arene Mesoporous Silica-Based HPLC Column

  • Original
  • Published:
Chromatographia Aims and scope Submit manuscript

Abstract

Mesoporous materials are described by their relatively high surface areas and pore volumes. They possess uniform channels within nanometer range. These materials have numerous applications in catalysis, separation and many other fields. The qualitative and quantitative determination of antibiotic drugs, i.e., ciprofloxacin and cefixime has clinical and analytical importance due to their broad spectrum of antimicrobial activity and stability. Both antibiotic drugs are orally active and have excellent activity against different pathogens. It is for the first time that we have developed an analytical method for the simultaneous analyses of both drugs using a newly developed p-morpholinomethylcalix[4]arene (p-MC4) mesoporous silica-based HPLC column (15 × 3 mm I.D.). Furthermore, separation of these two components was carried out using isocratic elution of methanol and 0.1% aqueous formic acid (70:30 v/v) with flow rate of 1 ml min−1 at retention time of 2.71 and 4.21 min and retention factor 1.85 and 1.19 for ciprofloxacin and cefixime, respectively; while total run time was 5 min. The developed method was repeatable with a relative standard deviation (RSD) of 0.90–2.08% for antibiotic drugs. The limits of detection and quantification of ciprofloxacin and cefixime were obtained within the range of 0.152–0.801 and 0.40–1.23 µg mL−1, respectively. The method is highly applicable, rapid, simple, very reproducible and accurate for the separation and determination of antibiotic drugs.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Scheme 1
Fig. 2
Fig. 3
Fig. 4

Similar content being viewed by others

References

  1. Abass K, Zafar I, Mohammad IK, Khalid J, Abad K, Lateef A, Yasar S, Fazli N (2011) Simultaneous determination of cefdinir and cefixime in human plasma by RP-HPLC/UV detection method: method development, optimization, validation, and its application to pharmaceutical study. J Chromatogr B 879:2423–2429

    Article  CAS  Google Scholar 

  2. Madan LM, Ayaz AM, Shahabuddin M, Fakhar NM, Ubed RM, Abdullah D, Naheed M, Mohammed AG, Mohammad KL (2015) Optimization of HPLC method for determination of cefixime using 2-thiophenecarboxaldehyde as derivatizing reagent: a new approach. Saudi Pharmaceutical J 23:444–452

    Article  Google Scholar 

  3. Troy DB, Beringer P (2005) Remingtons, the science and practice of pharmacy. 21st edn, vol 2, pp 1644, May 19, ISBN-10: 0781746736

  4. Sayed NHA, Bashir I, Nada SHA, Iman RSA, Noora ASA, Nafisur R (2013) Quantitative analysis of cefixime via complexation with palladium (II) in pharmaceutical formulation by spectrophotometry. J Pharm Anal 3:248–256

    Article  CAS  Google Scholar 

  5. Muhammad NQ, Inayat R, Gul AM (2012) Comparative analysis of ciprofloxacin in different pharmaceutical products by high performance liquid chromatography. Sci Tech Dev 31:69–73

    Google Scholar 

  6. Katzung B (2006) Basic and clinical pharmacology, (Chap. 8), Chemotherapeutic Drugs tenth ed., p 726, ISBN-10: 0071451536

  7. Shah J, Jan MR, Shah S, Inayatullah (2011) Spectrofluorimetric method for determination and validation of cefixime in pharmaceutical preparations through derivatization with 2-cyanoacetamide. J Fluoresc 21:579–585

    Article  CAS  PubMed  Google Scholar 

  8. Bukhari N, Al-Warthan A, Wabaidur SM, Othman ZA, Javid M, Haider S (2010) Spectrofluorimetric determination of cefi xime in pharmaceutical preparation and biological fluids using calcein as a fluorescence probe. Sens Lett 8:280–284

    Article  CAS  Google Scholar 

  9. Mendez JH, Perez AS, Zamarreno MD, Laso LV (1984) Differential pulse polarographic determination of Cephalexin based on the catalytic pre-wave of nickel (II). Anal Chim Acta 160:335–340

    Article  Google Scholar 

  10. Abdel Gaber AA, Farghaly OA, Ghandour MA, El-Said HS (2000) Potentiometric studies on some cephalosporin complexes. Monatsh Chem 131:1031–1038

    Article  Google Scholar 

  11. Fei Q, Li M, Wang B, Huan Y, Feng G et al (2009) Analysis of Cephalexine with NIR spectrometry coupled to artificial neural networks with modified genetic algorithm for wavelength selection. Chemometr Intell Lab 97:127–131

    Article  CAS  Google Scholar 

  12. Liu YM, Shi YM, Liu ZL (2010) Determination of enoxacin and ofl oxacin by capillary electrophoresis with electrochemiluminescence detection in biofl uids and drugs and its application to pharmacokinetics. Biomed Chromatogr 24:941–947

    Article  CAS  PubMed  Google Scholar 

  13. Sun Y, Tang Y, Yao H, Zheng X (2004) Potassium permanganate–glyoxal chemiluminescence system for flow injection analysis of cephalosporin antibiotics: cephalexine, cefadroxil, and cefazolin sodium in pharmaceutical preparations. Talanta 64:156–159

    Article  CAS  PubMed  Google Scholar 

  14. Andrasi M, Buglyo P, Zekany L, Gaspar A (2007) A comparative study of capillary zone electrophoresis and pH-potentiometry for determination of dissociation constants. J Pharm Biomed Anal 44:1040–1047

    Article  CAS  PubMed  Google Scholar 

  15. See KL, Elbashir AA, Saad B, Ali AS, Aboul-Enein HY (2009) Simultaneous determination of ofl oxacin and ornidazole in pharmaceutical preparations by capillary zone electrophoresis. Biomed Chromatogr 23:1283–1290

    Article  CAS  PubMed  Google Scholar 

  16. Attimarad MV, Alnajjar AO (2013) A conventional HPLC–MS method for the simultaneous determination of ofloxacin and cefixime in plasma: development and validation. J Basic Clinl Pharm 4:36–41

    Article  CAS  Google Scholar 

  17. Elias B, Alfeen A (2016) Determination of cefuroxime axetil and cefixime trihydrate in pharmaceutical dosage forms by RP-HPLC Method. Pharm Anal Chem 2:114

    Article  Google Scholar 

  18. Devika GS, Sudhakar M, Venkateshwara Rao J (2012) Simultaneous estimation of cefixime and moxifloxacin in bulk and its pharmaceutical dosage form by RP-HPLC. Orient J Chem 28:1743–1750

    Article  CAS  Google Scholar 

  19. Kavitha rani K, Harshini S, Sireesha D, Akiful haque M, Bakshi V. Padmanabha rao A (2014) Development and validation of analytical method for simultaneous estimation of cefixime and ofloxacin in bulk and tablet dosage form by rp-hplc method. Int J Pharma Res Health Sci 2:496–501

    CAS  Google Scholar 

  20. Gulderen U, Shahabuddin M, Mustafa Y (2001) Synthesis and binding properties of polymeric calix[4]arene nitriles. Reactive Funct Polym 50:77–84

    Google Scholar 

  21. Frank H, Maximilian C, Jurgen M, Michael F (2006) Silica-based mesoporous organic–inorganic hybrid materials. Angew Chem Int Ed 45:3216–3251

    Article  Google Scholar 

  22. Huayu H, Chuande Z, Yongsheng J, Rong N, Pan Z, Haixia Z (2010) Preparation, characterization and application of p-tert-butyl-calix[4]arene-SBA-15 mesoporous silica molecular sieves. J Hazard Mater 178:680–685

    Article  CAS  Google Scholar 

  23. Nasir V, Sadhana R (2011) Mesoporous material, MCM41: a new drug carrier. Asian J Pharm Clin Res 4:44–53

    Google Scholar 

  24. Zeid AA (2012) A review: fundamental aspects of silicate mesoporous materials materials. 5:2874–2902

  25. Gezici O, Tabakci M, Kara H, Yilmaz M (2006) Synthesis of p-tert-butylcalix[4]arene dinitrile bonded aminopropyl silica and investigating its usability as a stationary phase in HPLC. J Macro Sci Part A 43:221–231

    Article  CAS  Google Scholar 

  26. Fakhar NM, Ayyilidiz HF, Hüseyin K, Shahabuddin M, Adnan K, Muhammad KL, Mustafa T, Syed THS, Naeem AM, Fatih D, Ismail T (2015) Application of central composite design for the optimization of on-line solid phase extraction of Cu2+ by calix[4]arene bonded silica resin. Chemometr Intell Lab Syst 146:158–168

    Article  CAS  Google Scholar 

  27. Fatih D, Fakhar NM, Shahabuddin M, Ayaz AM, Naeem AM, Hüseyin K (2015) Copper sorption efficiency of p-tetranitrocalix[4]arene based high performance liquid chromatographic column. Desal Water Treat 1–7

  28. Gutsche CD, Stoddart JF (eds) (1998) Calixarenes Revisited. The Royal Society of Chemistry, England, Cambridge

    Google Scholar 

  29. Asli S, Begum T, Aydan Y (2012) Calix[4]arene-based Mannich and Schiff bases as versatile receptors for dichromate anion extraction: synthesis and comparative studies. Tetrahedron 68:8739–8745

    Article  CAS  Google Scholar 

  30. Erdemir S, Yilmaz M (2010) Preparation of a new 1,3-alternate-calix[4]arene-bonded HPLC stationary phase for the separation of phenols, aromatic amines and drugs. Talanta 82:1240–1246

    Article  CAS  PubMed  Google Scholar 

  31. ICH Q2 (R1) (2005) Validation of analytical procedure: text and methodology. International Conference on Harmonization, Geneva. http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines

Download references

Acknowledgements

The authors express gratitude to the National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro, Pakistan for supporting through financial support and providing the compulsory facilities.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Fakhar N. Memon.

Ethics declarations

Conflict of interest

The authors declare no conflict of interest.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Memon, N.A., Memon, A.A., Memon, F.N. et al. Method Development for Determination of Antibiotic Drugs Using Newly Prepared p-Morpholinomethylcalix[4]arene Mesoporous Silica-Based HPLC Column. Chromatographia 81, 1373–1380 (2018). https://doi.org/10.1007/s10337-018-3580-7

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10337-018-3580-7

Keywords

Navigation