Analysis and the determination of prednisolone in pharmaceutical products by a high-performance liquid chromatography method

Document Type : Original Article

Authors

1 Department of chemistry, Baghdad University College of science for women, Baghdad, Iraq

2 Department of Chemistry, Baghdad University College of Ibn al-Haithem, Baghdad, Iraq

3 College of Health and Medical Techniques, Almustaqbal University, Hilla, Iraq

Abstract
Prednisolone is essential because it is a potent corticosteroid medication with anti-inflammatory and immunosuppressive effects, widely used in both human and veterinary medicine. Therefore, accurate measurement is crucial for determining the correct human dose. A fast and high-performance liquid chromatography (HPLC) method was developed to determine prednisolone in both its pure form and pharmaceutical products. It consists of a 4.6 mm x 250 mm column (C18 packed with 5µm particles), with the mobile phase being (CH3OH: H2O) in a ratio of 58:42 v/v and a flow rate of 1 mL per minute, using an automatic injector (20 µL). The detection was performed at 254 nm with a UV detector. Detection of UV and Flow rate was obtained at 240–254 nm and 1.0 mL min-1.  Prednisolone is diluted in methanol or buffer before use. The retention time for prednisolone was found to be 8.383 minutes. The linearity range, LOD, and LOQ were obtained at 0.1-2 mg L-1, 0.029 mg L-1, and 0.098 mg L-1, respectively. Additionally, the working range of prednisolone is between 0.1 and 100 mg L-1 (RSD < 5%). The method showed good precision and accuracy, making it suitable for the quantification of prednisolone. The technique utilizes high sensitivity and selectivity, meeting regulatory requirements, and achieves a recovery rate of more than 95%.

Graphical Abstract

Analysis and the determination of prednisolone in pharmaceutical products by a high-performance liquid chromatography method

Keywords


D. Czock, F. Keller, FM. Rasche, U. Haussler, Pharmacokinetics and pharmacodynamics of systemically administered glucocorticoids, Clin. Pharmacokinet., 44 (2005) 61-98. http://dx.doi.org/10.2165/00003088-200544010-00003 
M. Pickup, Clinical pharmacokinetics of prednisone and prednisolone, Clin. Pharmacokinet., 4 (1979) 111-28. https://doi.org/10.2165/00003088-197904020-00004
J. Ferry, A. Horvath, Relative and absolute bioavailability of prednisone and prednisolone after separate oral and intravenous doses, J. Clin. Pharmacol., 28 (1988) 81-7. https://doi.org/10.1002/j.1552-4604.1988.tb03105
R. Kashyap, E. V. S. Subrahmanyam, A. R. Sharbaraya, Development and validation of UV spectroscopy method for the estimation of prednisolone in bulk and dosage form, J. Chem. Pharm. Res., 2 (2012) 1090-1096. https://www.jocpr.com/
C. Cardenas, P. Santhanam, Perioperative evaluation and management of patients on glucocorticoids, J. Endocr. Soc., 7 (2022) 185. https://doi.org/10.1210/jendso/bvac185
K. Bunte, D. Smith, M. Chappell, Learning pharmacokinetic models for in vivo glucocorticoid activation, J. Theor. Biol., 14 (2018) 222-231. https://doi.org/10.1016/j.jtbi.2018.07.025
F.I. Aljabari, H.M. Mashhhdani, M.J. Jehad, M. M. Kadhim, Synthesis and characterization of molecularly imprinted polymers for metronidazole by using allyl chloride and allyl bromide as monomer, Res. J. Pharm. Technol., 16 (2023) 715-720. https://doi.org/10.52711/0974-360X.2023.00122
M. Luaibi, K. Waleed, S. Al-Janabi, Development of a spectrophotometric determination of prednisolone in different dosage forms, Malay. J. Sci., 43 (2024) 30–36. https://doi.org/10.22452/mjs.vol43no3.4
S. Tabassum, M. Ajitha, Quantitative spectrophotometric estimation of prednisolone in tablet dosage form using eco-friendly green solvent and by applying Beer-Lambert’s law mathematical equation method, Asian J. Res. Chem., 14 (2021) 155. https://doi.org/10.52711/0974-4150.2021.00029   
S. Sura AL-Douri, Y. Shatha AL-Samarray, Spectrophotometric determination of prednisolone drug using cloud point extraction and pharmaceutical application, J. Pharm. Negative Results, 13 (2022) 189-197. https://doi.org/10.47750/pnr.2022.13.S01.23
J. Nasereddin, R. Al-Wadi, Optimization and validation of spectrophotometric methods for the determination of prednisolone in chitosan nanoparticles, J. Hunan Univ. Nat. Sci., 51 (2024) 83-91. https://doi.org/10.55463/issn.1674-2974.51.4.10
K. Vijaya, S. Shetty, Development and validation of UV spectrophotometric method for the estimation of methylprednisolone in bulk and pharmaceutical formulation, World J. Pharm.  Pharm. Sci., 7 (2018) 498-503. https://doi.org/10.32628/IJSRST24113116
G. Singh, D. Kumar, Q-Absorbance ratio spectrophotomertic method for the simultaneous estimation of prednislone and 5-amino salicylic acid tablet dosage form, Int. J. Appl. Pharm. Sci. Res., 2 (2012) 222- 226. https://doi.org/10.7324/JAPS.2012.2736
M. Rohitas, A. Agrawal, Development of simultaneous spectrophotometric method of mesalazine and prednisolone in same dosage form, Int. J. Appl. Pharm., 2 (2010) 8-11. https://doi.org/10.31032/IJBPAS/2023/12.6.1050
O. Bhusnure, M. Bawage, Eco-friendly and cost-effective UV spectroscopy method for the estimation of prednisolone sodium phosphate in bulk and pharmaceutical dosage form, Int. J. Pharm. Sci. Res., 6 (2014) 327-332. http://dx.doi.oP.rg/10.13040/IJPSR.0975-8232.6(1).327-32
M. Finšgar, A. Perva-Uzunalić, H. Behr, An Improved reversed-phase high-performance liquid chromatography method for the analysis of related substances of prednisolone in active ingredient, ACS Omega, 5 (2020) 7987–8000. https://doi.org/10.1021/acsomega.0c00037
O. Bhusnure,  S. Gholve, Analytical method development and validation of prednisolone sodium phoshphate by QBD approach, J. Pharm. Biol. Sci., 10 (2015) 64-75. https://doi.org/10.9790/3008-10636475
S. Ghosh, A. Sahu, Development and validation for prednisolone in tablet dosage form by reverse phase-HPLC, Asian J. Chem., 23 (2011) 5092-5094. https://hero.epa.gov/hero/index.cfm/reference/details/reference_id/1109763
M. Gai, E.  Pinllia, Determination of prednisolone and prednisone in plasma, whole blood, urine, and bound-to-plasma protein by high-performanceliquid chromatography, J. Chromatogr. Sci., 43 (2005) 201-206. https://doi.org/10.1093/chromsci/43.4.201
F. Aljabari, Y. AlBayati, Estimation of trimethoprim by using a new selective electrodes dependent on molecularly imprinted polymers, Egypt. J. Chem., 64 (2021) 6089-6096. https://doi.org/10.21608/EJCHEM.2021.72564.3617
F. I. Aljabari, Y. K. AlBayati. Synthesis and characterizations of a new Sulfamethoxazole-molecularly imprinted polymer and using for pharmaceutical application, AIP Conf. Proc., 2414 (2023) 050014. https://doi.org/10.1063/12.0013064
S. Teimoori, An immobilization of aminopropyl trimethoxysilane-phenanthrene carbaldehyde on graphene oxide for toluene extraction and separation in water samples, Chemosphere, 316 (2023) 137800. https://doi.org/10.1016/j.chemosphere.2023.137800
S. Teimoori, A. H. Hassani, M. Panahi, N. Mansouri, Rapid extraction of BTEX in water and milk samples based on functionalized MWCNTs by dispersive homogenized-micro-solid phase extraction, Food Chem., 421 (2023) 136229. https://doi.org/10.1016/j.foodchem.2023.136229
S. Teimoori, A. H. Hassani, New extraction of toluene from water samples based on nano-carbon structure before determination by gas chromatography, Int. J. Environ. Sci. Technol., 20 (2023) 6589–6608. https://doi.org/10.1007/s13762-023-04906-9
M. Mohammadi Asl, N. Mansouri, S. A. R. Haji Seyed Mirzahosseini, F. Atabi, Simultaneity comparative evaluation of toluene removal from the air by adsorption and UV semi-degradation-based adsorption procedure, Int. J. Environ. Sci. Technol., 21 (2024) 6677-6694. https://doi.org/10.1007/s13762-024-05503-0
M. Mohammadi Asl, Functionalized graphene oxide with bismuth and titanium oxide nanoparticles for efficiently removing formaldehyde from the air by photocatalytic degradation–adsorption process, J. Anal. Test., 7 (2023) 444-458. https://doi.org/10.1007/s41664-023-00272-0
R. Ashouri, S. A. R. Haji Seyed Mirzahosseini, N. Mansouri, Dynamic and static removal of benzene from air based on task-specific ionic liquid coated on MWCNTs by sorbent tube-headspace solid-phase extraction procedure, Int. J. Environ. Sci. Technol., 18 (2021) 2377-2390. https://doi.org/10.1007/s13762-020-02995-4
S. A. Hajiseyed Mirzahosseini, N. Mansouri, Synthesis of carbon quantum dots from olive stones for efficient adsorption of benzene from the ambient air, J. Nanostruct., 11 (2021) 480-497.  https://doi.org/10.22052/JNS.2021.03.007
A. Faghihi-Zarandi, J. Rakhtshah, B. B. Yarahmadi, A rapid removal of xylene vapor from environmental air based on bismuth oxide coupled to heterogeneous graphene/graphene oxide by UV photo-catalectic degradation-adsorption procedure, J. Environ. Chem. Eng., 8 (2020) 104193. https://doi.org/10.1016/j.jece.2020.104193
M. Aliomrani, M.A. Sahraian, Blood concentrations of cadmium and lead in multiple sclerosis patients from Iran, Iran. J. Pharm. Res., 15 (2016) 825-833. https://doi.org/10.22037/ijpr.2016.1941
A. Faghihi-Zarandi, H. Shirkhanloo, C. Jamshidzadeh, A new method for removal of hazardous toluene vapor from air based on ionic liquid-phase adsorbent, Int. J. Environ. Sci. Technol., 16 (2019) 2797-2808. https://doi.org/10.1007/s13762-018-1975-5
M. Arjomandi, H. Shirkhanloo, A review: analytical methods for heavy metals determination in environment and human samples, Anal. Methods Environ. Chem. J., 2 (2019) 97-126.  https://doi.org/10.24200/amecj.v2.i03
Y. Kamal Al-Bayati, F. Ibrahem Aljabari, Mefenamic acid selective membranes sensor and its application to pharmaceutical analysis, Baghdad Sci. J., 13 (2016) 829-637. https://doi.org/10.21123/bsj.2016.13.4.0829
J. Rakhtshah, N. Esmaeil, A rapid extraction of toxic styrene from water and wastewater samples based on hydroxyethyl methylimidazolium tetrafluoroborate immobilized on MWCNTs by ultra-assisted dispersive cyclic conjugation-micro-solid phase extraction Author links open overlay panel, Microchem. J., 170 (2021) 106759. https://doi.org/10.1016/j.microc.2021.106759
C. Jamshidzadeh, A new analytical method based on bismuth oxide-fullerene nanoparticles and photocatalytic oxidation technique for toluene removal from workplace air, Anal. Methods Environ. Chem. J., 2 (2019) 73-86. https://doi.org/10.24200/amecj.v2.i01.55
B. H. Abadi, H. Shirkhanloo, J. Rakhtshah, Air pollution control: The evaluation of TerphApm@ MWCNTs as a novel heterogeneous sorbent for benzene removal from air by solid phase gas extraction, Arabian J. Chem., 13 (2020) 1741-1751. https://doi.org/10.1016/j.arabjc.2018.01.011
H. Naseef, R. Moqadi, M. Qurt, Development and validation of an HPLC method for determination of antidiabetic drug alogliptin benzoate in bulk and tablets, J. Anal. Methods Chem., 24 (2018) 1902510. https://doi.org/1155/2018/1902510