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Screening and Optimization of the Reaction of Polymyxin B Sulphate with NBD-Cl for the Synchronous Spectrofluorimetric Determination of Polymyxin B Sulphate in Human Plasma

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Abstract

An accurate and sensitive synchronous spectrofluorimetric method has been developed for the determination of Polymyxin B sulphate (Poly B) in human plasma. The method is based on the reaction of non-fluorescent Poly B with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in borate buffer of pH 7 producing a yellow color with maximum relative fluorescence at 440 nm using a constant wavelength difference Δλ = 80 nm. Reaction conditions and other analytical parameters were studied and optimized using factorial design. Three level factorial designs have been employed for the screening, optimization of all experimental variables and determination of their interactions on the final product formation. The variables under investigation were: pH of borate buffer, volume of buffer, volume of NBD-Cl, temperature, time of heating and volume of sulfuric acid. A linear plot between relative fluorescence and concentration was obtained over the concentration range 100.00–1200.00 ng mL−1. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 10.31 and 31.24 ng mL−1, respectively. The proposed method was validated according to ICH guidelines and successfully applied for the determination of Poly B in human plasma, where satisfactory results were obtained. The results obtained were statistically compared with those of a published method, where no significant difference was observed.

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References

  1. Seth SD (2009) Textbook of pharmacology. Elsevier, India

    Google Scholar 

  2. Garidel P, Brandenburg K (2009) Current understanding of polymyxin B applications in bacteraemia/sepsis therapy prevention: clinical, pharmaceutical, structural and mechanistic aspects. Antiinfect Agents Med Chem 8:367–385

    Article  CAS  Google Scholar 

  3. Thomas AH, Holloway I (1978) Thin-layer chromatographic method for the identification of the polymyxins. J Chromatogr 161:417–420

    Article  CAS  Google Scholar 

  4. Krzek J, Starek M, Kwiecien A, Rzeszutko W (2001) Simultaneous identification and quantitative determination of neomycin sulfate, polymixin B sulfate, zinc bacitracin and methyl and propyl hydroxybenzoates in ophthalmic ointment by TLC. J Pharm Biomed Anal 24:629–636

    Article  CAS  PubMed  Google Scholar 

  5. Adams E, Schepers R, Gathu LW, Kibaya R, Roets E, Hoogmartens J (1997) Liquid chromatographic analysis of a formulation containing polymyxin, gramicidin and neomycin. J Pharm Biomed Anal 15:505–511

    Article  CAS  PubMed  Google Scholar 

  6. Orwa JA, Van Gerven A, Roets E, Hoogmartens J (2000) Liquid chromatography of polymyxin B sulphate. J Chromatogr A 870:237–243

    Article  CAS  PubMed  Google Scholar 

  7. Pendela M, Adams E, Hoogmartens J (2004) Development of a liquid chromatographic method for ear drops containing neomycin sulphate, polymyxin B sulphate and dexamethasone sodium phosphate. J Pharm Biomed Anal 36:751–757

    Article  CAS  PubMed  Google Scholar 

  8. Cao G, Ali FE, Chiu F, Zavascki AP, Nation RL, li J (2008) Development and validation of a reversed-phase high-performance liquid chromatography assay for polymyxin B in human plasma. J Antimicrob Chemother 62:1009–1014

    Article  CAS  PubMed  Google Scholar 

  9. Van den Bossche L, Van Schepdael A, Chopra S, Hoogmartens J, Adams E (2011) Identification of impurities in polymyxin B and colistin bulk sample using liquid chromatography coupled to mass spectrometry. Talanta 83:1521–1529

    Article  PubMed  Google Scholar 

  10. Thomas TA, Brown EC, Abildskov KM, Kubin CJ, Horan J, Yin MT, Cremers S (2012) High performance liquid chromatography-mass spectrometry (LC-MS) assay for polymyxin B1 and B2 in human plasma. Ther Drug Monit 34:398–405

    Article  PubMed Central  CAS  PubMed  Google Scholar 

  11. Haemers A, De Moerloose P (1970) The identification of polymyxin B sulphate. J Chromatogr 52:154–157

    Article  CAS  PubMed  Google Scholar 

  12. Gallego JML, Arroyo JP (2001) Simultaneous resolution of dexamethasone and polymyxin B by spectrophotometry derivative and multivariate methods. Anal Lett 34:1265–1283

    Article  CAS  Google Scholar 

  13. Gallego JML, Arroyo JP (2001) Spectrophotometric resolution of ternary mixtures of dexamethasone, polymyxin B and trimethoprim in synthetic and pharmaceutical formulations. Anal Chim Acta 437:247–257

    Article  Google Scholar 

  14. Srisom P, Liawruangrath B, Liawruangrath S, Slater JM, Wangkarn S (2007) Simultaneous determination of neomycin sulfate and polymyxin B sulfate by capillary electrophoresis with indirect UV detection. J Pharm Biomed Anal 43:1013–1018

    Article  CAS  PubMed  Google Scholar 

  15. Injac R, Linaric AM, Djorjevic-Milic V, Karljikovic K, Strukeli B (2008) Optimal condition for determination of zinc bacitracin, polymyxin B, oxytetracycline and sulfacetamide in Animal Feed by micellar electrokinetic capillary chromatography. Food Addit Contam Part A 25:424–431

    Article  CAS  Google Scholar 

  16. Gallego JML, Arroyo JP (2003) Determination of hydrocortisone, polymyxin B and Zn-bacitracin in pharmaceutical preparations by micellar electrokinetic chromatography. Anal Bioanal Chem 375:617–622

    CAS  PubMed  Google Scholar 

  17. Barnard JH (1984) Potency of polymyxin B1 and B2 fractions by turbidimetric assays and agar plate diffusion assay. Anal Proc 21:238–240

    CAS  Google Scholar 

  18. Jacobson M, Koch A, Kuntzman R (1984) The distribution and binding of tritiated polymyxin B in the mouse. J Pharmacol Exp Ther 183:433–439

    Google Scholar 

  19. Nevado JJB, Pulgarin JAM, Escudero OIR (2000) Determination of procaine and tetracaine in cocaine samples by variable-angle synchronous fluorimetry. Appl Spectrosc 54:1678–1683

    Article  CAS  Google Scholar 

  20. El-Enany N, Belal F, Rizk M (2006) Kinetic spectrophotometric determination of isoxsuprine in dosage forms through derivatisation with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl). Sci Pharm 74:99–119

    Article  CAS  Google Scholar 

  21. El-Enany N, Ahmid N, Belal F (2009) Spectrofluorimetric and spectrophotometric determination of oxamniquine in pharmaceuticals and biological fluids via derivatization with 4-Chloro-7-Nitrobenzo-2-oxa-1,3-Diazole (NBD-Cl). J Chin Chem Soc 56:485–492

    Article  CAS  Google Scholar 

  22. Merás ID, Dίaz TG, Franco MA (2005) Simultaneous fluorimetric determination of glyphosate and its metabolite, aminomethylphosphonic acid, in water, previous derivatization with NBD-Cl and by partial least squares calibration (PLS). Talanta 65:7–14

    Article  Google Scholar 

  23. Leitão JM, Esteves da Silva JC (2008) Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method. Anal Chim Acta 609:1–12

    Article  PubMed  Google Scholar 

  24. Persson-Stubberud K, Aström O (1998) Separation of ibuprofen, codeine phosphate, their degradation products and impurities by capillary electrophoresis: I. Method development and optimization with fractional factorial design. J Chromatogr A 798:307–314

    Article  CAS  PubMed  Google Scholar 

  25. Agatonović-Kuštrin S, Lj Ž, Vasiljević M, Radulović D (1997) Spectrophotometric study of diclofenac-Fe (III) complex. J Pharm Biomed Anal 16:147–153

    Article  PubMed  Google Scholar 

  26. Zavascki AP, Goldani LZ, Cao G, Superti SV, Lutz L, Barth AL, Ramos F, Boniatti MM, Nation RL, Li J (2008) Pharmacokinetics of intravenous polymyxin B in critically ill patients. Clin Infect Dis 47:1298–1304

    Article  CAS  PubMed  Google Scholar 

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Authors and Affiliations

  1. Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Organization of African Unity Street, Abassia, Cairo, 11566, Egypt

    A. M. El-Kosasy, Omar Abdel-Aziz, N. Magdy & N. M. El Zahar

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  1. A. M. El-Kosasy
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  2. Omar Abdel-Aziz
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  3. N. Magdy
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  4. N. M. El Zahar
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Correspondence to N. M. El Zahar.

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El-Kosasy, A.M., Abdel-Aziz, O., Magdy, N. et al. Screening and Optimization of the Reaction of Polymyxin B Sulphate with NBD-Cl for the Synchronous Spectrofluorimetric Determination of Polymyxin B Sulphate in Human Plasma. J Fluoresc 25, 695–705 (2015). https://doi.org/10.1007/s10895-015-1555-8

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  • DOI: https://doi.org/10.1007/s10895-015-1555-8

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