Research Journal of Pharmacy and Technology

Open Access Open Access  Restricted Access Subscription Access
Open Access Open Access Open Access  Restricted Access Restricted Access Subscription Access

Extractive Spectrophotometric Determination of Ulipristal Acetate using Naphthol Blue Black


Affiliations
1 Department of Chemistry, Acharya Nagarjuna University, Nagarjuna Nagar-522510, India
2 GITAM University – Bengaluru, Karnataka-562163, India
     

   Subscribe/Renew Journal


Ulipristal acetate is used to treat uterine fibroids and for emergency birth control. The present study is a first report on development of a visible spectrophotometric method for determination of Ulipristal acetate present in bulk and tablet formulation. The method involves the sequential addition of HCl (0.1 N) and Napthol Blue Black solution to Ulipristal acetate. Cation formed on tertiary amine group of Ulipristal acetate attracts anion of naphthol blue black (an acid dye) to develop a coloured ion-association complex. From the aqueous phase, the chromophore is extractable into chloroform, which exhibits λmax at 640 nm. As per the existing guidelines of ICH, various parameters of the method were tested for validation. Regression analysis (r > 0.999) shows that the plotted calibration curve exhibits good linearity in the studied range of concentration (2.50 – 15.00 μg mL-1). The % recovery values falls in 99.80 – 100.72 range. %RSD results of both precision studies were observed in the range 0.007 – 0.560, indicating the satisfactory precision of the method. Low values of R.S.D. (< 1 %) were observed indicating that the proposed method is reproducible, accurate and precise. The proposed method can be used in quality control laboratories for routine analysis of Ulipristal acetate (bulk drug and pharmaceutical dosage forms) without requirement of expensive instruments.

Keywords

Ulipristal Acetate, Naphthol Blue Black, Ion-Association Complex, Method Development, Validation.
Subscription Login to verify subscription
User
Notifications
Font Size


  • Attardi BJ, Burgenson J, Hild SA and Reel JR. In vitro antiprogestational/antiglucocorticoid activity and progestin and glucocorticoid receptor binding of the putative metabolites and synthetic derivatives of CDB-2914, CDB-4124, and mifepristone. The Journal of steroid biochemistry and molecular biology. 88(3); 2004:277-288.

  • Pohl O, Zobrist RH and Gotteland JP. The clinical pharmacology and pharmacokinetics of ulipristal acetate for the treatment of uterine fibroids. Reproductive Sciences. 22(4);2015:476-483.

  • Gainer EE and Ulmann A. Pharmacologic properties of CDB (VA)-2914. Steroids. 68(10-352 13);2003:1005-1011.

  • Fine P, Mathé H, Ginde S, Cullins V, Morfesis J and Gainer E. Ulipristal acetate taken 48–120 hours after intercourse for emergency contraception. Obstetrics &Gynecology. 115(2);2010: 257-263.

  • European Medicines Agency. Esmya (ulipristal acetate 5 mg tablets): EU summary of product characteristics. 2016. http:// www.ema.europa.eu/. Accessed 15 Mar 2017.

  • Garnock-Jones KP and Duggan ST. Ulipristal Acetate: A Review in Symptomatic Uterine Fibroids. Drugs. 77(15); 2017:1665-1675.

  • Bari AK, Prajapati PR, Modi VS And Desai SS. Development and validation of uv spectrometric method for quantitative determination of ulipristal acetate. International Journal of Pharmacy and Pharmaceutical Sciences. 7(7); 2015.

  • Pappula N, Kodali B and Datla PV. Rapid and sensitive determination of selective progesterone modulator ulipristal acetate in human plasma. European Journal of Chemistry.8(3);2017:258-264.

  • Nandakumar R, Praditpan P, Westhoff CL and Cremers S. A UPLC–MS/MS method for the quantitation of Ulipristal acetate in human serum. Journal of Chromatography B.1059;2017:43-48.

  • Béni Z, Orgoványi J, Kóti J, Sánta C, Horváth J, Mahó S and SzántayJr C. Detection by HPLC and structural characterization by NMR and MS of a natural deuterium isotopologue of ulipristal acetate. Journal of pharmaceutical and biomedical analysis. 98; 2014:279-286.

  • Gong A and Zhu X. Dispersive solvent-free ultrasound-assisted ionic liquid dispersive liquid–liquid microextraction coupled with HPLC for determination of ulipristal acetate. Talanta.131;2015:603-608.

  • Venkatarao M, Rao GS and Suresh D. Spectrophotometric determination of solifenacin succinate through ion association complex formation in bulk sample and pharmaceutical formulations. Asian Journal of Chemistry. 23(4);2011:1752-1754.

  • El Sherif ZA, Mohamed AO, Walash MI and Tarras FM. Spectrophotometric determination of loperamide hydrochloride by acid-dye and charge-transfer complexation methods in the presence of its degradation products. Journal of Pharmaceutical and Biomedical Analysis.22(1);2000:13-23.

  • Padmavathi M, Reshma MSR, Sindhuja YV, Venkateshwararao K Ch, and Naga Raju K. Spectrophotometric methods for estimation of telmisartan bulk drug and its dosage form. International Journal of Research in Pharmacy and Chemistry. 3(2); 2013: 320-325.

  • Krishna MV and Sankar DG. Spectrophotometric determination of gemifloxacin mesylate in pharmaceutical formulations through ion-pair complex formation. E-Journal of Chemistry.5(3); 2008:515-520.

  • Ashour S and Bayram R. Sensitive Extractional Colorimetric Analysis of Fexofenadine Hydrochloride and Irbesartan Bases Through Acid-Dye Complexation Using Naphthol Blue Black in Pure Form and Pharmaceuticals. Modern Chemistry.5(6); 2017:93-100.

  • Baba KH, Rambabu C, Rao KV, Khan RA and Rao KP. Assay of Dexmedetomidine in bulk samples and pharmaceutical formulations by extractive spectrophotometry. Chemical Science Transactions. 4(1);2015:270-274 . DOI:10.7598/cst2015.4624.

  • Begum J, Rao KS and Rambabu C. Assay of Yohimbine Chloride in Bulk Samples and Pharmaceutical Formulations by Extractive Spectrophotometry. Asian Journal of Chemistry. 18(2);2006:1417-1422.

  • Davidson AG, Beckett AH and Stenlake JB (eds.), Practical Pharmaceutical Chemistry, Part 2, Athalone Press, London. 1988: 304.

  • Sethi PD. HPLC quantitative analysis of pharmaceutical formulations.CBS publications, India, 2001.

  • ICH guidelines, Validation of Analytical Procedures. Text and Methodology. Q2 (R1); 2015: 8-13.

  • Kiran Kumar K, Venkata Nadh R and Nagoji KEV. Extractive Spectrophotometric Determination of Nicergoline Through Ion-pair Complexation Reaction. Oriental Journal of Chemistry 29 (1); 2013:263-269.

  • Sudhir MS and Nadh RV. Diazo-Coupling A Facile Mean for the Spectrophotometric Determination of Rasagiline Hemitartrate. Oriental Journal of Chemistry. 29(4);2014:1507-1514.

  • Kumar KK, Nadh RV and Nagoji KE. Determination of bendamustine hydrochloride in pure and dosage forms by ion-associative complex formation. Oriental Journal of Chemistry. 30(2); 2014:905-910.

  • Giri Prasad G and Venkata Nadh R, Oxidative Coupling: A Tranquil Approach for Determination of Selexipag by Visible Spectrophotometry, Oriental Journal of Chemistry 34(6); 2018; 3112-3117. DOI: 10.13005/ojc/340656.

  • Giri Prasad G and Venkata Nadh R, Determination of mianserine using Fe3+-phenanthroline by visible spectrophotometry, Research Journal of Pharmacy and Technology. 34(6); 2018; 3112-3117. DOI: 10.13005/ojc/340656.


Abstract Views: 140

PDF Views: 0




  • Extractive Spectrophotometric Determination of Ulipristal Acetate using Naphthol Blue Black

Abstract Views: 140  |  PDF Views: 0

Authors

Giri Prasad Gorumutchu
Department of Chemistry, Acharya Nagarjuna University, Nagarjuna Nagar-522510, India
Venkata Nadh Ratnakaram
GITAM University – Bengaluru, Karnataka-562163, India

Abstract


Ulipristal acetate is used to treat uterine fibroids and for emergency birth control. The present study is a first report on development of a visible spectrophotometric method for determination of Ulipristal acetate present in bulk and tablet formulation. The method involves the sequential addition of HCl (0.1 N) and Napthol Blue Black solution to Ulipristal acetate. Cation formed on tertiary amine group of Ulipristal acetate attracts anion of naphthol blue black (an acid dye) to develop a coloured ion-association complex. From the aqueous phase, the chromophore is extractable into chloroform, which exhibits λmax at 640 nm. As per the existing guidelines of ICH, various parameters of the method were tested for validation. Regression analysis (r > 0.999) shows that the plotted calibration curve exhibits good linearity in the studied range of concentration (2.50 – 15.00 μg mL-1). The % recovery values falls in 99.80 – 100.72 range. %RSD results of both precision studies were observed in the range 0.007 – 0.560, indicating the satisfactory precision of the method. Low values of R.S.D. (< 1 %) were observed indicating that the proposed method is reproducible, accurate and precise. The proposed method can be used in quality control laboratories for routine analysis of Ulipristal acetate (bulk drug and pharmaceutical dosage forms) without requirement of expensive instruments.

Keywords


Ulipristal Acetate, Naphthol Blue Black, Ion-Association Complex, Method Development, Validation.

References