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A validated RP-HPLC method for determination of nitroxinil and investigation of its intrinsic stability

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Abstract

A fast, sensitive and selective RP-HPLC method was developed for extensive investigation of nitroxinil’s stability. The stability of the studied drug was tested under different stress conditions, namely hydrolytic, oxidative, photolytic and thermal. Separation of nitroxinil and its degradation products was achieved in less than 5 min using Venusil XBP C18 (150 × 2.1 mm id, 5 um particle size) column and isocratic mobile phase composed of 0.1% triethylamine pH 2.5 (adjusted with phosphoric acid) and acetonitrile mixture in a ratio of (70:30; v/v). UV detection at 270 nm was employed for monitoring nitroxinil degradation behavior over a linearity range of 1–75 µg/mL. Plackett–Burman experimental design was adopted for robustness testing of the developed chromatographic method. LC-mass identification of nitroxinil’s hydrolytic and oxidative degradations was attempted, and the suggested mechanism was deduced. The proposed method was successfully applied in determination of the drug in raw material and pharmaceutical dosage form.

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References

  1. A.C. Moffat, M.D. Osselton, B. Widdop, J. Watts, Clarke’s analysis of drugs and poisons, in Pharmaceuticals, Body Fluids and Postmortem Material, 4th. Pharmaceutical Press (2011)

  2. British Pharmacopeia, Her Majesty’s Stationary Office, London, UK (2016)

  3. W.J. Blanchflower, D.G. Kennedy, Determination of nitroxynil residues in tissues using high-performance liquid chromatography-thermospray mass spectrometry. Analyst 114, 1013–1015 (1989)

    Article  CAS  Google Scholar 

  4. J.A. Tarbin, G. Shearer, High-performance liquid chromatographic method for the determination of the anthelmintic nitroxynil in cattle muscle tissue with on-line anion-exchange clean-up. J. Chromatogr. 613, 347–353 (1993)

    Article  CAS  Google Scholar 

  5. M. Sakamoto, K. Takeba, T. Sasamoto et al., Determination of bithionol, bromophen, nitroxynil, oxyclozanide, and tribromsalan in milk with liquid chromatography coupled with tandem mass spectrometry. J AOAC Int 93, 1340–1346 (2010)

    Article  CAS  Google Scholar 

  6. M. Whelan, Y. Bloemhoff, A. Furey et al., Investigation of the persistence of nitroxynil residues in milk from lactating dairy cows by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry. J. Agric. Food Chem. 59, 7793–7797 (2011). https://doi.org/10.1021/jf202050r

    Article  CAS  PubMed  Google Scholar 

  7. K. Takeba, M. Matsumoto, Determination of nitroxynil in cow milk by reversed-phase high-performance liquid chromatography with dual- electrode coulometric detection. J. Chromatogr. 596, 67–71 (1992)

    Article  CAS  Google Scholar 

  8. G. Shearer, Short Communication liquid chromatographic method for the determination of the anthelmintic nitroxynil in cattle muscle tissue with on-line anion-exchange. 3, 347–353 (1993)

  9. M. Caldow, M. Sharman, M. Kelly et al., Multi-residue determination of phenolic and salicylanilide anthelmintics and related compounds in bovine kidney by liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 1216, 8200–8205 (2009). https://doi.org/10.1016/j.chroma.2009.04.008

    Article  CAS  PubMed  Google Scholar 

  10. K.M. Cooper, M. Whelan, M. Danaher et al., Stability during cooking of anthelmintic veterinary drug residues in beef. Food Addit. Contam. 28, 155 (2012). https://doi.org/10.1080/19440049.2010.542775

    Article  CAS  Google Scholar 

  11. Sunil Kumar Yelamanchi, Useni Reddy Mallu, I.V. Kasi Viswanath, G.N. Murthy, RP-HPLC method development and validation for nitroxynil in active Pharmaceutical ingredient. J Pharm Sci researh 8, 967–973 (2016)

    CAS  Google Scholar 

  12. M.M. Ghoneim, M. El-ries, A.M. Hassanein, A.M. Abd-elaziz, Voltammetric assay of the anthelmintic veterinary drug nitroxynil in bulk form and formulation at a mercury electrode. J. Pharm. Biomed. Anal. 41, 1268–1273 (2006). https://doi.org/10.1016/j.jpba.2006.03.022

    Article  CAS  PubMed  Google Scholar 

  13. I.M. Traynor, C.S. Thompson, L. Armstrong et al., Determination of nitroxynil residues in tissues and bovine milk by immunobiosensor. Food Addit Contam Part A 30, 1115–1122 (2013). https://doi.org/10.1080/19440049.2013.781274

    Article  CAS  Google Scholar 

  14. (2016) United State Pharmacopeia and National Formulary (USP39—NF34). Rockville,MD,

  15. Speeding up your HPLC. http://www.chromacademy.com/chromatography-speeding-up-your-HPLC.html. Accessed 25 Mar 2017

  16. Chemicalize. https://chemicalize.com/#/calculation. Accessed 25 Mar 2017

  17. ReviewerGuidance, Validation of Chromatographic Methods, Center for Drug Evaluation and Research(CDER),FDA,. Rockville, MD (1994)

  18. Y. Qiu, Y. Chen, L. Yu, R.V. Mantril, Developing Oral Dosage forms pharmaceutical theory and practice, 2nd edn. (Academic Press, Boca Raton, 2016)

    Google Scholar 

  19. F.A. Carey, R.J. Sundberg, Advanced Organic Chemistry, 5th edn. (Springer, Berlin, 2007)

    Google Scholar 

  20. J.E. Mcissac Jr., R.E. Bal Jr, E.J. Behrman, The mechanism of the base catalyzed conversion of nitrile to amides by hydrogen peroxide. J. Org. Chem. 3961, 3048–3050 (1971)

    Article  Google Scholar 

  21. J. Ermer, J.H.M. Miller, Method validation in pharmaceutical analysis: A guide to best practice, first edit (WILEY-VCH Verlag GmbH & Co, KGaA, Weinheim, 2005)

    Book  Google Scholar 

  22. Y. Vander Heyden, A. Nijhuis, J. Nijhuis et al., Guidance for robustness/ruggedness tests in method validation. J. Pharm. Biomed. Anal. 24, 723–753 (2001). https://doi.org/10.1016/S0731-7085(00)00529-X

    Article  CAS  PubMed  Google Scholar 

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Acknowledgment

The research was carried out using the materials, equipment and facilities of National Organization for Drug Control and Research, Ministry of Health, Egypt.

Funding

This research did not receive any specific grant from funding agencies in the public, commercial or not-for-profit sectors.

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Authors and Affiliations

  1. National Organization of Drug Control and Research (NODCAR), 51 Wezzart Elzeraa Street, Elagouza, Giza12618, Egypt

    Marwa Soliman & Nahla Sayed Ismail

  2. Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr ElـAini Street, Cairo, 11562, Egypt

    Ahmed Sayed Saad & Hala El-sayed Zaazaa

Authors
  1. Marwa Soliman
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  2. Ahmed Sayed Saad
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  3. Nahla Sayed Ismail
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  4. Hala El-sayed Zaazaa
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Correspondence to Marwa Soliman.

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Soliman, M., Saad, A.S., Ismail, N.S. et al. A validated RP-HPLC method for determination of nitroxinil and investigation of its intrinsic stability. J IRAN CHEM SOC 18, 351–361 (2021). https://doi.org/10.1007/s13738-020-02030-w

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  • DOI: https://doi.org/10.1007/s13738-020-02030-w

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