RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE COMBINATION OF IMIQUIMOD AND SALICYLIC ACID

ANKITA SHARMA; INDER KUMAR; KARAN RANA

doi:10.22159/ijpps.2020v12i9.38382

Authors

ANKITA SHARMA Department of Pharmaceutical Chemistry, Abhilashi College of Pharmacy, Nerchwok, Mandi, HP, India
INDER KUMAR Department of Pharmaceutics, School of Pharmacy, Abhilashi University, Mandi, HP, India
KARAN RANA Quality Control Executive, Complex Pharma, Karnal, Haryana, India

DOI:

https://doi.org/10.22159/ijpps.2020v12i9.38382

Keywords:

Imiquimod, Salicylic acid, Reverse-phase high-performance liquid chromatography (RP-HPLC), Validation, International council for harmonization (ICH)

Abstract

Objective: The present study was undertaken to develop and validate an RP-HPLC method for the combination of imiquimod and salicylic acid

Methods: The method was carried out on Nucleodur C18 (250 mm × 4.6 mm I.D., 5 ????m) using low-pressure gradient elution mode. The mobile phase was used as 30M potassium dihydrogen phosphate and acetonitrile (45:55) pH 6.5 adjusted using ortho-phosphoric acid. The concentration of solvents was 1-20 µg/ml and the volume of injection was 20 mcl with the flow rate of 1.0 ml/min. The absorption maxima of salicylic acid and imiquimod were found 234 nm and 226 nm, respectively.

Results: The method was validated and showed the linearity greater than 0.99% and with precision (RSD%<1). The limit of detection (LOD) and limit of quantification (LOQ) of salicylic acid was found to be 0.09756 µg/ml and 0.2956 µg/ml, respectively, and imiquimod was found to be 0.044031 µg/ml and 0.13334 µg/ml, respectively.

Conclusion: The method developed in the present study was found to be sensitive, specific, and can be applied for the simultaneous estimation of imiquimod and salicylic acid.

Downloads

Download data is not yet available.

References

Paula DD, Martins CA, Bentley MV. Development and validation of HPLC method for imiquimod determination in skin penetration studies. Biomed Chromatography 2008;22: 1416-23.

Hussain S, Shaikh T, Farooqui M. Development and validation of liquid chromatography method for the determination and quantification of impurities in imiquimod. J Pharm Res Int 2016;3:1-9.

Jain S, Diwan A, Sardana S. Development and validation of UV spectroscopy and RP-HPLC methods for estimation of imiquimod. Int J Pharm Sci Rev Res 2015;35:16-21.

Tyring SK, Rosen T. Beyond a decade of 5% imiquimod topical therapy. J Drugs Dermatol 2009;8:467-74.

Madan RK, Levitt J. A review of toxicity from topical salicylic acid preparations. J Am Acad Dermatol 2014;70:788-92.

Bruner CR, Feldman SR, Ventrapragada M, Fleischer AB. A systematic review of adverse effects associated with topical treatments for psoriasis. Dermatol Online J 2003;9:2.

Scotter MJ, Roberts DP, Wilson LA, Howard FA, Davis J, Mansell N. Free salicylic acid and acetylsalicylic acid content of foods using gas chromatography-mass spectrometry. Food Chem 2007;105:273-9.

Ekinci D, Şentürk M, Kufrevioglu OI. Salicylic acid derivatives: synthesis, features and usage as therapeutic tools. Expert Opin Ther Pat 2011;21:1831-41.

Chitlange SS, Imran M, Sakarkar DM. RP-HPLC method for simultaneous estimation of amlodipine and metoprolol in tablet formulation. Asian J Pharm 2008;2:232-4.

Kokot Z, Burda K. Simultaneous determination of salicylic acid and acetylsalicylic acid in aspirin delayed-release tablet formulations by second-derivative UV spectrophotometry.

J Pharm Biomed Anal 1998;18(4 Suppl 5):871-5.

Guideline IH. Validation of analytical procedures: text and methodology Q2 (R1). International conference on harmonization, Geneva, Switzerland; 2005. p. 1-13.

Perlatti B, Maria Fd, Graças FdS, Fernandes JB, Ross M. Validation and application of HPLC–ESI-MS/MS method for the quantification of RBBR decolorization, a model for highly toxic molecules, using several fungi strains. Bio-Tech 2012; 124:37–44.

Krier F, Michael B, Benjamin D, Pierre L, Aurelie D, Eric Z, et al. Optimisation and validation of a fast HPLC method for the quantification of sulindac and its related impurities. J Pharmaceut Biomed Anal 2011;54:694–70.

Gonzalez O, Iriarte G, Ferreiros N, Maguregui MI, Alonso RM, Jimenez RM. Optimization and validation of a SPE-HPLCPDA-fluorescence method for the simultaneous determination of drugs used in combined cardiovascular therapy in human plasma. J Pharmaceut Biomed 2009;50:630–9.

ICH Q2 (R1). Validation of analytical procedures: text and methodology. International Conference on Harmonization, IFPMA, Geneva; 2005.

Tranfo G, Enrico P, Renata S, Daniela P. Validation of an HPLC/MS/MS method with isotopic dilution for quantitative determination of trans, trans-muconic acid in urine samples of workers exposed to low benzene concentrations. J Chromatogr Biomed 2008;867:26–30.

Jenke DR. Chromatographic method validation: a review of current practices and procedures. Part II. Guidelines for primary validation parameters. Instrum Sci Technol 1998; 26:1-18.

Staes E, Rozet E, Ucakar B, Hubert P, Preat V. Validation of a method for the quantitation of ghrelin and unacylated ghrelin by HPLC. J Pharmaceut Biomed Anal 2010;51:633-9.

Patel BD, Bhavya Mehta, Chaudhary B Ankit. Method development and validation for simultaneous estimation of lamivudine and zidovudine in tablet by reverse-phase high-performance liquid chromatography. Asian J Pharm Clin Res 2020;13:73-7.

Rajan D Senthil, G Muruganathan, Shivkumar Kumutaavall, Thangavel Ganesh. Development and validation of hplc method for simultaneous quantification of vasicine, glycyrrhizin and piperine in poly herbal cough syrup. Int J Curr Pharm Res 2020;12:15-9.

Trani MTT, Katherine MP, Marlyn C. Matrix-specific method validation for quantitative analysis of vitamin C in diverse foods. J Food Compost Anal 2012;26:12–25.

Hernandez YS, Sanchez LB, Bedia MMG, Luis TG. Determination of parthenin in Parthenium hysterophorus by means of HPLC-UV: method development and validation. Phytochem Lett 2011;4:134.