Abstract
A novel, rapid, and sensitive stability-indicating high-performance thin-layer chromatography method was developed and validated for the simultaneous determination of celecoxib (CEL) and diacerein (DIA) in bulk and a capsule binary mixture. The complete separation was achieved by the proposed method on nanosilica gel F254 plates using n-hexane‒ethyl acetate‒tetrahydrofuran‒glacial acetic acid (7:3:1:0.8, V/V) as the mobile phase. The chromatographic bands were visualized using short-wave ultraviolet light, and the amount of CEL and DIA was determined by scanning densitometry at 254 nm using the peak area. The RF values were 0.59 and 0.37 for CEL and DIA, respectively. From regression plots, it was found that good linearity was achieved in the concentration ranges of 20.00–320.00 ng/band and 5.00–80.00 ng/band with mean percentage recoveries 99.86 ± 0.70 and 99.64 ± 0.96 for CEL and DIA, respectively. The proposed method was validated according to the International Conference on Harmonisation guidelines. The statistical analysis of the results revealed high accuracy and precision, the suggested procedures could be used as a stability-indicating assay for the simultaneous determination of CEL and DIA in bulk drug and their capsule binary mixture in the presence of their degradation products.
Similar content being viewed by others
Abbreviations
- CEL:
-
Celecoxib
- DIA:
-
Diacerein
- THF:
-
Tetrahydrofuran
- SD:
-
Standard deviation
- RSD:
-
Relative standard deviation
- SE:
-
Standard error
- R F :
-
Retention factor
- LOQ:
-
Limit of quantification
- LOD:
-
Limit of detection
References
British Pharmacopoeia (2019) Vol. 1. Medicines and Healthcare Products Regulatory Agency, London
The United States Pharmacopeia and National Formulary (2016) The official compendia of standards, Asian Edition, USP 39-NF34 The United States Pharmacopeial Conversion Inc., Rockvill, MD
Ong CKS, Lirk P, Tan CH, Seymour RA (2007) An evidence-based update on nonsteroidal anti-inflammatory drugs. Clin Med Res 5:19–34
Howard PA, Delafontaine P (2004) Nonsteroidal anti-inflammatory drugs and cardiovascular risk. J Am Coll Cardiol 43:519–525
Ali H, Nawab A, Farooq N, Ashraf I, Sodagar M, Tariq A, Naqvi GR (2018) Celecoxib as an effective Cox-2 inhibitor for rheumatologic disorders: efficacy and safety concerns. AJSMU 4(1):51–56
Tanaka A, Araki H, Komoike Y, Hase S, Takeuchi K (2001) Inhibition of both COX-1 and COX-2 is required for development of gastric damage in response to nonsteroidal anti inflammatory drugs. J Physiol Paris 95:21–27
Mahajan A, Singh K, Tandon VR, Kumar S, Kumar H (2006) Diacerein: a new symptomatic slow acting drug for osteoarthritis. JK Sci 8(3):173–175
Douni E, Sfikakis PP, Haralambous S, Fernandes P, Kollias G (2004) Research article attenuation of inflammatory polyarthritis in TNF transgenic mice by diacerein: comparative analysis with dexamethasone, methotrexate and anti-TNF protocols. Arthritis Res Ther 6(1):65–72
Dalal B, Kubavat A, Kshatriya RR (2012) A randomized, active controlled, clinical trial to assess the efficacy and safety of celecoxib + diacerein fixed dose combination in adult Indian patients suffering from osteoarthritis. IJMHS 2(2):31–34
Attimarad M, Venugopala KN, Aldhubiab BE, Nair AB, Sree Harsha N, Pottathil S et al (2019) Development of UV spectrophotometric procedures for determination of amlodipine and celecoxib in formulation: use of scaling factor to improve the sensitivity. J Spectrosc 2019:1–10
Kaur D, Kaur J, Kamal SS (2019) Development and validation of a UV spectrophotometric method for determination of diacerein in bulk and a capsule dosage form. Indian J Pharm Sci 81(1):124–128
Damiani P, Bearzotti M, Cabezón MA (2003) A validated spectrofluorometric method for the determination of celecoxib in capsules. Anal Bioanal Chem 376(7):1141–1146
Baboota S, Shakeel F, Ahuja A, Ali J, Shafiq S, Ahmad S (2007) Development and validation of a stability-indicating HPLC method for analysis of celecoxib (CXB) in bulk drug and microemulsion formulations. Acta Chromatogr 18:116
Raghava Raju TV, Kumar SR, Srinivas A, Kumar NA, Rao IM, Rao NS (2014) Development and validation of a stability-indicating RP-HPLC method for the estimation of diacerein impurities in API and pharmaceutical formulation. J Liq Chromatogr Relat Technol 37(4):498–515
Rao J, Chauhan K, Mahadik KR, Kadam SS (2009) A stability-indicating high performance liquid chromatographic method for the determination of diacerein in capsules. Indian J Pharm Sci 71(1):24–29
Ali NW, Abdelwahab NS, Abdelkawy M, Emam AA (2014) Validated stability indicating TLC–densitometric method for the determination of diacerein. J Chromatogr Sci 52(1):5–11
Sane RT, Pandit S, Khedkar S (2004) High-performance thin-layer chromatographic determination of celecoxib in its dosage form. J Planar Chromatogr 17(1):61–64
Gandhi S, Dewani M, Borole TC, Damle MC (2012) Development and validation of stability indicating HPTLC method for determination of diacerein and aceclofenac as bulk drug and in tablet dosage form. E-J Chem 9(4):2023–2028
ArkanE KarimiZ, ShamsipurM SaberR (2013) Electrochemical determination of celecoxib on a graphene based carbon ionic liquid electrode modified with gold nanoparticles and its application to pharmaceutical analysis. Anal Sci 29(8):855–860
PatelNS NandurbarkarVP, PatelAJ PatelSG (2014) Simultaneous spectrophotometric determination of celecoxib and diacerein in bulk and capsule by absorption correction method and chemometric methods. Spectrochim Acta, Part A 125:46–52
Bapatu HR, Maram RK, Murthy RS (2015) Stability-indicating HPLC method for quantification of celecoxib and diacerein along with its impurities in capsule dosage form. J Chromatogr Sci 53(1):144–153
ICH (2005) Validation of analytical procedures: text and methodology Q2 (R1). In: International conference on harmonization. IFPMA, Geneva
Variyar PS, Chatterjee S, Sharma A (2011) Fundamentals and theory of HPTLC-based separation. In: Srivastava MM (ed) High-performance thin-layer chromatography (HPTLC). Springer, Berlin, pp 27–39
Miller J, Miller JC (2018) Statistics and chemometrics for analytical chemistry, 4th edn. Pearson Prentice Hall, Harlow
Acknowledgements
Not applicable.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declared that they have no competing interests.
Electronic supplementary material
Below is the link to the electronic supplementary material.
Rights and permissions
About this article
Cite this article
Rizk, M.M.S., Toubar, S.S., Gadallah, E.R.A. et al. A Rapid and reliable thin-layer chromatographic method for the simultaneous estimation of celecoxib and diacerein in their binary mixture using nanosilica gel plate. JPC-J Planar Chromat 33, 511–522 (2020). https://doi.org/10.1007/s00764-020-00064-7
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00764-020-00064-7