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Current Pharmaceutical Analysis

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ISSN (Print): 1573-4129
ISSN (Online): 1875-676X

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Research Article

Development and Validation of RP-HPLC Method for the Simultaneous Determination of Levamisole HCl and Oxyclozanide and its Application in the Assay of Veterinary Bolus Formulations

Author(s): Kemal Hussien Seid, Tarekegn Berhanu, Kaleab Asres and Ayenew Ashenef*

Volume 17, Issue 5, 2021

Published on: 11 February, 2020

Page: [679 - 689] Pages: 11

DOI: 10.2174/1573412916666200211101633

Price: $65

Abstract

Introduction: A reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous analysis of two drugs, levamisole hydrochloride (LH) and oxyclozanide (OX), in co-formulation for veterinary use.

Materials and Methods: The new HPLC method was validated as per the ICH and other guidelines. A C18 column was used with a gradient program; eluent A was an equal mixture of methanol and acetonitrile, and eluent B included a 25 mM phosphate buffer at pH 7.0 containing 30 mM sodium decanesulfonate and triethylamine (50:50:1 v/v) with pH adjusted to 7.0 using H3PO4 [51:49 v/v] .The detection wavelength was set at 220 nm. For the final gradient program, the retention times were 8.2(for LH) and 13.6(for OX) minutes, respectively, at a flow rate of 1 ml/min over 20 minutes run time.

Results: The method was precise, specific and robust. The correlation coefficient, R2 was 0.9998 and 0.9999 for LH and OX, respectively in the range of 5 – 280 μg / mL. The percent y-intercepts and percent residual standard deviations were 1.6%/0.4% and 1.4%/1.0% for LH and OX, respectively. The LOD and LOQ of the method were 0.21 μg / mL and 0.62 μg / mL for LH and 0.06 μg / mL and 0.18 μg / mL for OX. The method has an average accuracy of 100.5% for LH and 101.1% for OX when tested on veterinary bolus formulations, and the samples could be stored under typical lab conditions for about 7 days without significant degradation.

Conclusion: This HPLC method is suitable for assaying levamisole hydrochloride and oxyclozanide simultaneously from veterinary formulations.

Keywords: Analytical method development, bolus formulations, RP-HPLC, levamisole, oxyclozanide, imidazothiazole.

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[1]
Dreassi, E.; Corbini, G.; La Rosa, C.; Politi, N.; Corti, P. Determination of levamisole in animal tissues using liquid chromatography with ultraviolet detection. J. Agric. Food Chem., 2001, 49(12), 5702-5705.
[http://dx.doi.org/10.1021/jf0102362] [PMID: 11743750]
[2]
Bishop, Y. The Veterinary Formulary, Six Edition; Pharmaceutical Press: London/ UK, 2005, pp. 194-199.
[3]
Broome, A.W.; Jones, W.G.M. A new drug for the treatment of fascioliasis in sheep and cattle. Nature, 1966, 210(5037), 744-745.
[http://dx.doi.org/10.1038/210744a0] [PMID: 6006650]
[4]
USP-30 NF-27 In: National Formulary and the official compendia of standards; Port city press: Baltimore/USA. , 2007.
[5]
British Pharmacopoeia (veterinary) (2004); London, 2004, pp. 63, 70, 69, 124-125, 130..
[6]
European Pharmacopoeia, 5th ed; Council of Europe: Strasbourg, 2008, pp. 2253-2255.
[7]
British Pharmacopoeia; The Stationary Office, 2009, Vol. II, pp. 1152-1154, 1368-1369.
[8]
El-Kholy, H.; Kemppainen, B.W. Liquid chromatographic method with ultraviolet absorbance detection for measurement of levamisole in chicken tissues, eggs and plasma. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 2003, 796(2), 371-377.
[http://dx.doi.org/10.1016/j.jchromb.2003.08.025] [PMID: 14581076]
[9]
Dolezalová, M.; Tkaczyková, M. LC determination of the enantiomeric purity of levamisole using stationary phase with bonded naphthylethylcarbamoylated-β-cyclodextrin. J. Pharm. Biomed. Anal., 2001, 25(3-4), 407-415.
[http://dx.doi.org/10.1016/S0731-7085(00)00513-6] [PMID: 11377020]
[10]
Cholifah, S.; Kartinasari, W.F.; Indrayanto, G. Simultaneous HPLC determination of levamisole hydrochloride and anhydrous niclosamide in veterinary powders, and its validation. J. Liq. Chromatogr. Relat. Technol., 2008, 31, 281-291.
[http://dx.doi.org/10.1080/10826070701739132]
[11]
Cherlet, M.; De Baere, S.; Croubels, S.; De Backer, P. Quantitative analysis of levamisole in porcine tissues by high-performance liquid chromatography combined with atmospheric pressure chemical ionization mass spectrometry. J. Chromatogr. B Biomed. Sci. Appl., 2000, 742(2), 283-293.
[http://dx.doi.org/10.1016/S0378-4347(00)00171-7] [PMID: 10901133]
[12]
De Baere, S.; Cherlet, M.; Croubels, S.; Baert, K.; De Backer, P. Liquid chromatographic determination of levamisole in animal plasma: ultraviolet versus tandem mass spectrometric detection. Anal. Chim. Acta, 2003, 483, 215-224.
[http://dx.doi.org/10.1016/S0003-2670(02)01377-6]
[13]
Tong, L.; Ding, L.; Li, Y.; Wang, Z.; Wang, J.; Liu, Y.; Yang, L.; Wen, A. A sensitive LC-MS/MS method for determination of levamisole in human plasma: application to pharmacokinetic study. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 2011, 879(5-6), 299-303.
[http://dx.doi.org/10.1016/j.jchromb.2010.11.015] [PMID: 21256094]
[14]
Sadeghi, S.; Fathi, F.; Abbasifar, J. Potentiometric sensing of levamisole hydrochloride based on molecularly imprinted polymer. J. Sensor Actuator B, 2007, 122, 158-164.
[http://dx.doi.org/10.1016/j.snb.2006.05.018]
[15]
Khalil, S.; Borham, N. Indirect atomic absorption spectrometric determination of pindolol, propranolol and levamisole hydrochlorides based on formation of ion-associates with ammonium reineckate and sodium cobaltinitrite. J. Pharm. Biomed. Anal., 2000, 22(2), 235-240.
[http://dx.doi.org/10.1016/S0731-7085(99)00269-1] [PMID: 10719905]
[16]
El Ries, M.A.; Khalil, S. Indirect atomic absorption determination of atropine, diphenhydramine, tolazoline, and levamisole based on formation of ion-associates with potassium tetraiodometrcurate. J. Pharm. Biomed. Anal., 2001, 25(1), 3-7.
[http://dx.doi.org/10.1016/S0731-7085(00)00459-3] [PMID: 11274852]
[17]
Khalil, S.; El-Rabiehi, M.M. Indirect atomic absorption spectrometric determination of pindolol, propranolol and levamisole hydrochlorides based on formation of ion associates with manganese thiocyanate and potassium ferricyanide. J. Pharm. Biomed. Anal., 2000, 22(1), 7-12.
[http://dx.doi.org/10.1016/S0731-7085(99)00240-X] [PMID: 10727118]
[18]
Kumar, A.R.; Shetty, S.A.K. Development and validation of RP-HPLC method for the estimation of oxyclozanide in bulk drug and pharmaceutical formulations. Int. J. Chemtech Res., 2012, 4(2), 700-704.
[19]
Jo, K.; Cho, H.J.; Yi, H.; Cho, S.M.; Park, J.A.; Kwon, C.H.; Park, H.R.; Kwon, K.S.; Shin, H.C. Determination of oxyclozanide in beef and milk using high-performance liquid chromatography system with uv detector. Lab. Anim. Res., 2011, 27(1), 37-40.
[http://dx.doi.org/10.5625/lar.2011.27.1.37] [PMID: 21826158]
[20]
Tonder, E.C.; Villiers, M.M.; Handford, J.S.; Malan, C.E.P.; Preez, J.L. Simple, robust and accurate high-performance liquid chromatography method for the analysis of several anthelmintics in veterinary formulations. J. Chromatogr. A, 1996, 729, 267-272.
[http://dx.doi.org/10.1016/0021-9673(95)01253-2]
[21]
Whelan, M.; Chirollo, C.; Furey, A.; Cortesi, M.L.; Anastasio, A.; Danaher, M. Investigation of the persistence of levamisole and oxyclozanide in milk and fate in cheese. J. Agric. Food Chem., 2010-a, 58(23), 12204-12209.
[http://dx.doi.org/10.1021/jf102725b] [PMID: 21058728]
[22]
Whelan, M.; Kinsella, B.; Furey, A.; Moloney, M.; Cantwell, H.; Lehotay, S.J.; Danaher, M. Determination of anthelmintic drug residues in milk using ultra high performance liquid chromatography-tandem mass spectrometry with rapid polarity switching. J. Chromatogr. A, 2010, 1217(27), 4612-4622.
[http://dx.doi.org/10.1016/j.chroma.2010.05.007] [PMID: 20564781]
[23]
Kinsella, B.; Lehotay, S.J.; Mastovska, K.; Lightfield, A.R.; Furey, A.; Danaher, M. New method for the analysis of flukicide and other anthelmintic residues in bovine milk and liver using liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta, 2009, 637(1-2), 196-207.
[http://dx.doi.org/10.1016/j.aca.2008.10.072] [PMID: 19286030]
[24]
Jedziniak, P.; Szprengier-Juszkiewicz, T.; Olejnik, M. Determination of benzimidazoles and levamisole residues in milk by liquid chromatography-mass spectrometry: screening method development and validation. J. Chromatogr. A, 2009, 1216(46), 8165-8172.
[http://dx.doi.org/10.1016/j.chroma.2009.07.036] [PMID: 19656518]
[25]
Rasmussen, HT; Li, W.; Redlich, D.; Jimidar, M I HPLC Method Development in Hand Books of Pharmaceutical Analysis by HPLC; Elsevier Academic Press: Amesterdam The Netherlands, 2005, p. PP177..
[26]
Snyder, L.R.; Kirkland, J.J.; Glajch, J.L. , 1997, Practical HPLC Method Development, 2nd Edition;; 1-20.
[http://dx.doi.org/10.1002/9781118592014]
[27]
Jimidar, M.I.; Heylen, P.; De Smet, M. Method Validation in HPLC Method Development for Pharmaceuticals, 1st ed; Elsevier Academic Press: London, UK, 2007, pp. 441-457.
[http://dx.doi.org/10.1016/S0149-6395(07)80022-5]
[28]
Karen, M.A.; Robert, T.C.F.; Todd, D.H.; Linda, L.L.; Thomas, R.S.; Kimberly, D.S.; Edward, J.S. Degradation and Impurity Analysis for Pharmaceutical drug candidates in Handbook of Modern Pharmaceutical Analysis; Academic Press: San Diego, USA, 2001, Vol. 3, pp. 98-101.
[29]
Patel, T.; LoBrutto, R. John Wiley & Sons, Inc.: New Jersey, 2007, pp. Method validation in HPLC for Pharmaceutical Scientists, first Edition; 211, 455-487. .
[30]
Port city press: Baltimore/USA, 2009, 2, pp. National Formulary and the official compendia of standards, Validation of compendial procedures, USP (2009) 26 edn; 2218-222..
[31]
Birrer, G.A.; Murthy, S.S.; Liu, J.; Estrada, J. Parentral Dosage Forms in Hand Books of modern Pharmaceutical Analysis; Academic Press: San Diego, USA, 2001, Vol. 3, p. 276.
[32]
Ornaf, R.M.; Dong, M.W. Key Concepts in Pharmaceutical Analysis.In: Hand Book of Pharmaceutical Analysis By HPLC, 1st ed; Elsevier Inc: London, 2005, p. 29.
[http://dx.doi.org/10.1016/S0149-6395(05)80046-7]
[33]
Chan, C.C.; Lee, Y.C.; Lam, H.; Zhang, X. Analytical method validation and instrument performance verification; John Wiley and Sons, Inc.: New Jersey, USA, 2004, pp. 14-27-49, 73-75. http://dx.doi.org/10.1002/0471463728..

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