Whiter and Greener RP-HPLC Method for Simultaneous Determination of Dorzolamide, Brinzolamide, and Timolol Using Isopropanol as a Sustainable Organic Solvent in the Mobile Phase

Sami El Deeb; Khalid Abdelsamad; Maria Kristina Parr

doi:10.3390/separations11030083

journal article Open Access Mar 12, 2024

Whiter and Greener RP-HPLC Method for Simultaneous Determination of Dorzolamide, Brinzolamide, and Timolol Using Isopropanol as a Sustainable Organic Solvent in the Mobile Phase

Sami El Deeb

Khalid Abdelsamad Maria Kristina Parr

Separations Vol. 11 No. 3 pp. 83 · MDPI AG

View at Publisher Save 10.3390/separations11030083

Abstract

A sustainable reversed-phase chromatographic method has been developed and validated for the simultaneous determination of three active pharmaceutical ingredients, dorzolamide, brinzolamide, and timolol, used to treat glaucoma. The eco-friendly solvent isopropanol has been used as an organic mobile phase constituent. According to the Hansen space green solvent selection tool, isopropanol has a G score of 6.5, comparable to ethanol, which has a G score of 6.6. The mobile phase consists of isopropanol: aqueous sodium acetate buffer (0.1 M, pH 4.25) in the ratio of 10:90 (v/v). The flow rate was maintained at 1 mL/min. Dorzolamide and brinzolamide were detected at 254 nm, and timolol was detected at 295 nm. A high-purity silica with a polymeric C18 modification column (150 × 4.6 mm, 5 µm particle size) was used for this separation. The three compounds were eluted within 8 min. The method was validated according to ICH guidelines. The calibration curves were linear in the range of 20–70 µg/mL, 40–140 µg/mL, and 20–70 µg/mL for dorzolamide, brinzolamide, and timolol, respectively. The LODs were found to be 1.61 µg/mL, 1.60 µg/mL, and 3.16 µg/mL for dorzolamide, brinzolamide, and timolol, respectively. Good accuracy and precision were obtained for the three compounds. The greenness and whiteness of the method were indicated using the AGREE, ChlorTox, and RGB12 tools.

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References

45

[1]

Anastas "Green chemistry" Frontiers (1998)

[2]

The 12 principles of green analytical chemistry and the SIGNIFICANCE mnemonic of green analytical practices

Agnieszka Gałuszka, Zdzisław Migaszewski, Jacek Namieśnik

TrAC Trends in Analytical Chemistry 2013 10.1016/j.trac.2013.04.010

[3]

Migaszewski "Analytical eco-scale for assessing the greenness of analytical procedures" TrAC Trends Anal. Chem. (2012) 10.1016/j.trac.2012.03.013

[4]

(2024, January 08). National Environmental Methods Index, Available online: www.nemi.gov.

[5]

Sancho "A new tool for evaluating and/or selecting analytical methods: Summarizing the information in a hexagon" TrAC Trends Anal. Chem. (2019) 10.1016/j.trac.2019.06.015

[6]

A new tool for the evaluation of the analytical procedure: Green Analytical Procedure Index

J. Płotka-Wasylka

Talanta 2018 10.1016/j.talanta.2018.01.013

[7]

Hicks "Making the move towards modernized greener separations: Introduction of the analytical method greenness score (AMGS) calculator" Green Chem. (2019) 10.1039/c8gc03875a

[8]

AGREE—Analytical GREEnness Metric Approach and Software

Francisco Pena-Pereira, Wojciech Wojnowski, Marek Tobiszewski

Analytical Chemistry 2020 10.1021/acs.analchem.0c01887

[9]

Nowak "How to evaluate methods used in chemical laboratories in terms of the total chemical risk?—A ChlorTox Scale" Green Anal. Chem. (2023) 10.1016/j.greeac.2023.100056

[10]

Nowak "White analytical chemistry: An approach to reconcile the principles of green analytical chemistry and functionality" TrAC Trends Anal. Chem. (2021) 10.1016/j.trac.2021.116223

[11]

Blue applicability grade index (BAGI) and software: a new tool for the evaluation of method practicality

Natalia Manousi, Wojciech Wojnowski, Justyna Płotka-Wasylka et al.

Green Chem. 2023 10.1039/d3gc02347h

[12]

(2024, January 08). Blue Applicability Grade Index (BAGI). Available online: https://bagi-index.anvil.app/.

[13]

Hussain "White analytical chemistry approaches for analytical and bioanalytical techniques: Applications and challenges" TrAC Trends Anal. Chem. (2023) 10.1016/j.trac.2022.116905

[14]

(2020). Step ICH Guideline Q3C (R8) on Impurities: Guideline for Residual Solvents, European Medicines Agency.

[15]

CHEM21 selection guide of classical- and less classical-solvents

Denis Prat, Andy Wells, John Hayler et al.

Green Chem. 2016 10.1039/c5gc01008j

[16]

Tools and techniques for solvent selection: green solvent selection guides

Fergal P. Byrne, Saimeng Jin, Giulia Paggiola et al.

Sustainable Chemical Processes 2016 10.1186/s40508-016-0051-z

[17]

Aslamaci, A., Saat, B., and Aşlamacı, A. (2024, January 08). GREEN ELECTROSPINNING Making Electrospinning Environmentally Friendly. Available online: https://doi.org/10.13140/RG.2.2.33115.13603.

[18]

Larsen "A tool for identifying green solvents for printed electronics" Nat. Commun. (2021) 10.1038/s41467-021-24761-x

[19]

(2024, February 01). Isopropanol Safety Data Sheet. Available online: https://www.sigmaaldrich.com/RO/En/sds/SIAL/W292912?userType=undefined.

[20]

Nuzzi "Glaucoma: Biological trabecular and neuroretinal pathology with perspectives of therapy innovation and preventive diagnosis" Front. Neurosci. (2017) 10.3389/fnins.2017.00494

[21]

Nuzzi "What is new in glaucoma: From treatment to biological perspectives" J. Ophthalmol. (2021) 10.1155/2021/5013529

[22]

Bourne "Causes of vision loss worldwide, 1990–2010: A systematic analysis" Lancet Glob. Health (2013) 10.1016/s2214-109x(13)70113-x

[23]

The number of people with glaucoma worldwide in 2010 and 2020

H A Quigley

British Journal of Ophthalmology 2006 10.1136/bjo.2005.081224

[24]

Lee "Glaucoma and its treatment: A review" Am. J. Health Pharm. (2005) 10.1093/ajhp/62.7.691

[25]

Michaud "Comparison of topical brinzolamide 1% and dorzolamide 2% eye drops given twice daily in addition to timolol 0.5% in patients with primary open-angle glaucoma or ocular hypertension" Am. J. Ophthalmol. (2001) 10.1016/s0002-9394(01)00974-6

[26]

Ingram "Effect of brinzolamide and dorzolamide on aqueous humor flow in human eyes" Am. J. Ophthalmol. (1999) 10.1016/s0002-9394(99)00179-8

[27]

Balfour "Dorzolamide" Drugs Aging (1997) 10.2165/00002512-199710050-00006

[28]

Sugrue "Review the preclinical pharmacology of dorzolamide hydrochloride, a topical carbonic anhydrase inhibitor" J. Ocul. Pharmacol. Ther. (1996) 10.1089/jop.1996.12.363

[29]

National Center for Biotechnology Information (2023, November 02). PubChem Compound Summary for CID 5284549, Dorzolamide, Available online: https://pubchem.ncbi.nlm.nih.gov/compound/dorzolamide.

[30]

Iester "Brinzolamide" Expert Opin. Pharmacother. (2008) 10.1517/14656566.9.4.653

[31]

National Center for Biotechnology Information (2023, November 02). PubChem Compound Summary for CID 68844, Brinzolamide, Available online: https://pubchem.ncbi.nlm.nih.gov/compound/brinzolamide.

[32]

Narendra "Validated LC method for the estimation of dorzolamide HCl (carbonic anhydrase inhibitor) in ophthalmic solutions" J. Chem. (2012) 10.1155/2012/258261

[33]

Thangabalan "New RP-HPLC method development and validation for dorzolamide in ophthalmic dosage form" J. Anal. Methods Chem. (2018) 10.1155/2018/4596141

[34]

Tiwari "Analytical method development and validation for the determination of Brinzolamide by RP-HPLC" J. Drug Deliv. Ther. (2020) 10.22270/jddt.v10i1.3845

[35]

"Analytical quality by design development of an ecologically acceptable enantioselective HPLC method for timolol maleate enantiomeric purity testing on ovomucoid chiral stationary phase" J. Pharm. Biomed. Anal. (2020) 10.1016/j.jpba.2019.113034

[36]

Mohamed "Simultaneous determination of dorzolomide and timolol in aqueous humor: A novel salting out liquid–liquid microextraction combined with HPLC" Talanta (2014) 10.1016/j.talanta.2014.06.074

[37]

Annapurna, M.M., Narendra, A., and Deepika, D. (2012). Development and validation of RP-HPLC method for simultaneous determination of dorzolamide and timolol maleate in pharmaceutical dosage forms. J. Drug Deliv. Ther., 2. 10.22270/jddt.v2i2.120

[38]

Erk "Rapid and sensitive HPLC method for the simultaneous determination of dorzolamide hydrochloride and timolol maleate in eye drops with diode-array and UV detection" Pharmazie (2003)

[39]

Mandour, A.A., Nabil, N., Zaazaa, H.E., Ibrahim, M.M., and Ibrahim, M.A. (2023). Two stability indicating chromatographic methods: TLC densitometric versus HPLC method for the simultaneous determination of brinzolamide and timolol maleate in ophthalmic formulation in the presence of probable carcinogenic oxidative degradation product of timolol maleate. Separations, 10. 10.3390/separations10010037

[40]

Mandour "Review on analytical studies of some pharmaceutical compounds containing heterocyclic rings: Brinzolamide, timolol maleate, flumethasone pivalate, and clioquinol" Future J. Pharm. Sci. (2020) 10.1186/s43094-020-00068-4

[41]

Abd-AlGhafar, W.N., Aly, F.A., Sheribah, Z.A., and Saad, S. (2022). Green HPLC method with time programming for the determination of the co-formulated eye drops of tafluprost and timolol in their challengeable ratio. BMC Chem., 16. 10.1186/s13065-022-00815-z

[42]

Ibrahim "A versatile HPLC method with an isocratic single mobile phase system for simultaneous determination of anti-glaucoma formulations containing timolol" Ann. Pharm. Françaises (2019) 10.1016/j.pharma.2019.02.005

[43]

Hassib "Simultaneous determination of timolol maleate in combination with some other anti-glaucoma drugs in rabbit aqueous humor by high performance liquid chromatography–tandem mass spectroscopy" J. Chromatogr. B (2016) 10.1016/j.jchromb.2016.04.012

[44]

(2023, November 02). Available online: https://green-solvent-tool.herokuapp.com/.

[45]

International Conference on Harmonization Geneva (2005). ICH Guideline for Validation of Analytical Procedure: Text and Methodology, Q2 (R1), ICH. Available online: https://database.ich.org/sites/default/files/Q2%28R1%29%20Guideline.pdf.

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Details

Published: Mar 12, 2024
Vol/Issue: 11(3)
Pages: 83
License: View

Authors

S

Sami El Deeb

Institute of Pharmacy, Freie Universität Berlin, Königin-Luise-Str. 2+4, 14195 Berlin, Germany; Institute of Medicinal and Pharmaceutical Chemistry, Technische Universität Braunschweig, Beethoven-Str. 5, 38106 Braunschweig, Germany

K

Khalid Abdelsamad

Institute of Pharmacy, Freie Universität Berlin, Königin-Luise-Str. 2+4, 14195 Berlin, Germany

M

Maria Kristina Parr

Institute of Pharmacy, Freie Universität Berlin, Königin-Luise-Str. 2+4, 14195 Berlin, Germany

Cite This Article

Sami El Deeb, Khalid Abdelsamad, Maria Kristina Parr (2024). Whiter and Greener RP-HPLC Method for Simultaneous Determination of Dorzolamide, Brinzolamide, and Timolol Using Isopropanol as a Sustainable Organic Solvent in the Mobile Phase. Separations, 11(3), 83. https://doi.org/10.3390/separations11030083

Whiter and Greener RP-HPLC Method for Simultaneous Determination of Dorzolamide, Brinzolamide, and Timolol Using Isopropanol as a Sustainable Organic Solvent in the Mobile Phase

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