Solid Phase Extraction and Simultaneous Chromatographic Quantification of some Non-steroidal Anti-inflammatory Drug Residues
an Application in Pharmaceutical Industrial Wastewater Effluent
DOI:
https://doi.org/10.1590/s2175-97902022e18691Keywords:
Non-steroidal anti-inflammatory drugs, HPLC, Wastewater, TLC, SPEAbstract
Two sensitive and selective methods were developed for the simultaneous determination of four commonly used non-steroidal anti-inflammatory drugs (NSAIDs), namely; paracetamol (PCM), diclofenac sodium (DCF), ibuprofen (IBP), and indomethacin (IND) in wastewater effluents. The first method used HPLC for the determination of the studied drugs using a mobile phase consisting of phosphate buffer (pH 3.0) and acetonitrile at a flow rate of 1 mL/min. in gradient elution mode and detection at 220 nm. The separation process was performed on BDS Hypersil Cyano column (250 x 4.6 mm, 5 μm). The second method was a TLC-densitometric one which was performed using n-Hexane: ethyl acetate: acetic acid in the ratio (6:3.5:0.5) as a developing system. The proposed chromatographic methods were successfully applied for the selective determination of the four studied drugs in simulated and real pharmaceutical wastewater samples after their solid-phase extraction.
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Alsirawan MB, Mohammad MA, Alkasmi B, Alhareth K, El-Hammadi M. Development and validation of a simple HPLC method for the determination of ibuprofen sticking onto punch faces. Int J Pharm Pharm Sci. 2013;5(4):227-31.
Bouissou-Schurtz C, Houeto P, Guerbet M, Bachelot M, Casellas C, Mauclaire A-C, et al. Ecological risk assessment of the presence of pharmaceutical residues in a French national water survey. Regulatory Toxicology and Pharmacology [Internet]. Academic Press; 2014. Aug 1 [cited 2019 Mar 11];69(3):296-303. Available from: Available from: https://www.sciencedirect.com/science/article/pii/S0273230014000695
» https://www.sciencedirect.com/science/article/pii/S0273230014000695
Brooks BW, Turner PK, Stanley JK, Weston JJ, Glidewell EA, Foran CM, et al. Waterborne and sediment toxicity of fluoxetine to select organisms. Chemosphere. 2003;52(1):135-42.
Castello M, Pais N, De Souza Nascimento E. Guideline values and human risk assessment for the presence of anti-inflammatory drugs remaining in drinking water after lab scale treatment. J. Pharm. Sci [Internet]. 2018 [cited 2019 Mar 8];54(1):17320. Available from: Available from: http://dx.doi.org/10.1590/s2175-97902018000117320
» http://dx.doi.org/10.1590/s2175-97902018000117320
Crane M, Watts C, Boucard T. Chronic aquatic environmental risks from exposure to human pharmaceuticals. Sci Total Environ. 2006;367(1):23-41.
Devi TAP, Setti A, Srikanth S, Nallapeta S, Pawar SC, Rao JV. Original article Method development and validation of paracetamol drug by RP-HPLC. J Med Allied Sci. 2013;3(1):8-14.
Fadhil Ali K, Rasool Mahmood Albakaa A, Hussein Ali Z. New assay method UV spectroscopy for determination of Indomethacin in pharmaceutical formulation. J Chem Pharm Res. 2015;7(4):1591-1596.
Farid NF, Abdelaleem EA. HPTLC Method for the Determination of Paracetamol, Pseudoephedrine, and Loratidine in Tablets and Human Plasma. Journal of chromatographic science [Internet]. Oxford University Press; 2016 Apr [cited 2016 Oct 18];54(4):647-652. Available from: Available from: http://www.ncbi.nlm.nih.gov/pubmed/26762956
» http://www.ncbi.nlm.nih.gov/pubmed/26762956
Gaworecki KM, Klaine SJ. Behavioral and biochemical responses of hybrid striped bass during and after fluoxetine exposure. Aquat Toxicol. 2008;88(4):207-213.
Gómez MJ, Petrović M, Fernández-Alba AR, Barceló D. Determination of pharmaceuticals of various therapeutic classes by solid-phase extraction and liquid chromatography-tandem mass spectrometry analysis in hospital effluent wastewaters. J Chromatogr A. 2006;1114(2):224-233.
Hoeger B, Köllner B, Dietrich DR, Hitzfeld B. Water-borne diclofenac affects kidney and gill integrity and selected immune parameters in brown trout (Salmo trutta f. fario). Aquat Toxicol . 2005;75(1):53-64.
Ibrahim HK, Abdel-Moety MM, Abdel-Gawad SA, Al-Ghobashy MA, Kawy MA. Validated electrochemical and chromatographic quantifications of some antibiotic residues in pharmaceutical industrial wastewater. Environmental Science and Pollution Research [Internet]. Springer Berlin Heidelberg; 2017 Mar 14 [cited 2018 Jan 24];24(8):7023-7034. Available from: Available from: http://link.springer.com/10.1007/s11356-016-8340-3
» http://link.springer.com/10.1007/s11356-016-8340-3
Kidd D. International Conference on Harmonization. International Conference on Harmonization [Internet]. 1996 [cited 2016 Nov 1];4(1):183-206. Available from: Available from: http://www.ich.org/home.html
» http://www.ich.org/home.html
Kreisberg J. Ecological healing and the web of life. EXPLORE: The Journal of Science and Healing [Internet]. Elsevier; 2005 Mar [cited 2017 Feb 24];1(2):133-135. Available from: Available from: http://linkinghub.elsevier.com/retrieve/pii/S1550830704000242
» http://linkinghub.elsevier.com/retrieve/pii/S1550830704000242
Lindner E˝, Umezawa Y. Performance evaluation criteria for preparation and measurement of macro- and micro fabricated ion selective electrodes. Pure Appl. Chem. 2008;80(1):85-104.
Mathew M, Ashokan AS, Puthusseri S. Development and validation of UV spectrophotometric methods for simultaneous estimation of tolperisone hydrochloride and diclofenac sodium in tablet dosage form. International Journal of Pharmacy and Biological Sciences [Internet]. 2013 [cited 2016 Oct 18];3(4):42-48. Available from: Available from: www.ijpbs.com
» www.ijpbs.com
Matin AA, Farajzadeh MA, Jouyban A. A simple spectrophotometric method for determination of sodium diclofenac in pharmaceutical formulations. Il Farmaco. 2005;60(10):855-858.
Mervartová K, Polášek M, Calatayud JM. Sequential injection analysis (SIA)-chemiluminescence determination of indomethacin using tris[(2,2′-bipyridyl)]ruthenium(III) as reagent and its application to semisolid pharmaceutical dosage forms. Analytica Chimica Acta. 2007;600(1):114-121.
Moffat AC, Osselton MD, Widdop B, Watts J. Clarke’s analysis of drugs and poisons. Fourth Edi.. 2011.
Nakov N, Petkovska R, Ugrinova L, Kavrakovski Z, Dimitrovska A, Svinarov D. Critical development by design of a rugged HPLC-MS/MS method for direct determination of ibuprofen enantiomers in human plasma. Journal of Chromatography B. 2015;992:67-75.
Nentwig G. Effects of Pharmaceuticals on Aquatic Invertebrates. Part II: The Antidepressant Drug Fluoxetine. Archives of Environmental Contamination and Toxicology [Internet]. Springer-Verlag; 2007 Feb 7 [cited 2017 Feb 24];52(2):163-170. Available from: Available from: http://link.springer.com/10.1007/s00244-005-7190-7
» http://link.springer.com/10.1007/s00244-005-7190-7
Olajire AA, Olakunle SI, Ajibola AO. Novel colorimetric assay of indomethacin using 4-carboxyl-2,6-dinitrobenzene diazonium ion. Acta Pharm. 2006;56:189-202.
Panusa A, Multari G, Incarnato G, Gagliardi L. High-performance liquid chromatography analysis of anti-inflammatory pharmaceuticals with ultraviolet and electrospray-mass spectrometry detection in suspected counterfeit homeopathic medicinal products. Journal of Pharmaceutical and Biomedical Analysis. 2007;43(4):1221-1227.
Pavan Kumar SR, Bhuvan Kumar G, Sekhar TC, Murthy SB. Spectrophotometric Determination of Paracetamol Using Sodium bismuthate as Chromogen. Int. J. Res. Chem. Environ. International Journal of Research in Chemistry and Environment. 2012;2(2):231-235.
Pomati F, Castiglioni S, Zuccato E, Fanelli R, Vigetti D, Rossetti C, et al. Effects of a complex mixture of therapeutic drugs at environmental levels on human embryonic cells. Environmental science & technology [Internet]. 2006 Apr 1 [cited 2017 Feb 24];40(7):2442-7. Available from: Available from: http://www.ncbi.nlm.nih.gov/pubmed/16646487
» http://www.ncbi.nlm.nih.gov/pubmed/16646487
Pomati F, Netting AG, Calamari D, Neilan BA. Effects of erythromycin, tetracycline, and ibuprofen on the growth of Synechocystis sp. and Lemna minor. Aquatic Toxicol. 2004;67(4):387396.
Quinn B, Gagné F, Blaise C. An investigation into the acute and chronic toxicity of eleven pharmaceuticals (and their solvents) found in wastewater effluent on the cnidarian, Hydra attenuata. Sci Total Environment. 2008;389(2): 306-314.
Rockville. The Pharmacopoeia of the United States - National Formulary USP 39-NF 34 [Internet]. 2015 [cited 2017 Mar 31]. Available from: Available from: http://www.pharmacopeia.cn/v29240/usp29nf24s0_c621_viewall.html
» http://www.pharmacopeia.cn/v29240/usp29nf24s0_c621_viewall.html
Şahin S, Demir C, Güçer Ş. Simultaneous UV-vis spectrophotometric determination of disperse dyes in textile wastewater by partial least squares and principal component regression. Dyes Pigm. 2007;73(3):368-376.
Santini AO, de Oliveira JE, Pezza HR, Pezza L. A new potentiometric ibuprofenate ion sensor immobilized in a graphite matrix for determination of ibuprofen in tablets. Microchem J. 2006;84(1):44-49.
Spangenberg B, Poole CF, Weins C. Theoretical Basis of Thin Layer Chromatography (TLC). Quantitative Thin-Layer Chromatography [Internet]. Berlin, Heidelberg: Springer Berlin Heidelberg; 2010 [cited 2017 Mar 31]. p. 13-52. Available from: Available from: http://link.springer.com/10.1007/978-3-642-10729-0_2
» http://link.springer.com/10.1007/978-3-642-10729-0_2
Stanley JK, Ramirez AJ, Chambliss CK, Brooks BW. Enantiospecific sublethal effects of the antidepressant fluoxetine to a model aquatic vertebrate and invertebrate. Chemosphere . 2007;69(1):9-16.
Swaroopa Rani GN. Polarographic determination of Paracetamol by Calibration method using Fuchsin and different supporting electrolytes. Int Res J Sci Eng. 2015;3(34):156-165.
Sweetman SC. The Complete Drug Reference [Internet]. 36th editi. London,United Kingdom: Pharmaceutical Press; 2014 [cited 2018 Jan 25]. Available from: Available from: https://www.abe.pl/html/files/2014047-DMO-Martindale_2014.pdf
» https://www.abe.pl/html/files/2014047-DMO-Martindale_2014.pdf
Szeitz A, Edginton AN, Peng HT, Cheung B, Riggs KW. A Validated Enantioselective Assay for the Determination of Ibuprofen in Human Plasma Using Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry (UPLC-MS/MS). Am J Anal Chem [Internet]. Scientific Research Publishing; 2010 [cited 2016 Oct 18];01(02):47-58. Available from: Available from: http://www.scirp.org/journal/PaperDownload.aspx?DOI=10.4236/ajac.2010.12007
» http://www.scirp.org/journal/PaperDownload.aspx?DOI=10.4236/ajac.2010.12007
The British Pharmacopoeia Commission Secretariat of the Medicines and Healthcare Products Regulatory Agency (MHRA). British Pharmacopeia. I,II. London,United Kingdom: (The Stationery Office); 2015.
Turiel E, Bordin G, Rodríguez AR. Determination of quinolones and fluoroquinolones in hospital sewage water by off-line and on-line solid-phase extraction procedures coupled to HPLC-UV. J Sep Sci [Internet]. WILEY-VCH Verlag; 2005 [cited 2016 Oct 18];28(3):257-267. Available from: Available from: http://doi.wiley.com/10.1002/jssc.200400018
» http://doi.wiley.com/10.1002/jssc.200400018
Vemula V, Sharma P. Gradient High Performance Liquid Chromatography Method Development and Validation for Simultaneous Determination of Phenylephrine and Ibuprofen in Tablet Dosage Form. Trop J Pharm Res [Internet]. Faculty of Pharmacy, University of Benin; 2014 [cited 2016 Oct 18];13(6):967-974. Available from: Available from: http://www.ajol.info/index.php/tjpr/article/view/107722
» http://www.ajol.info/index.php/tjpr/article/view/107722
Vera-Candioti L, Gil García MD, Martínez Galera M, Goicoechea HC. Chemometric assisted solid-phase microextraction for the determination of anti-inflammatory and antiepileptic drugs in river water by liquid chromatography-diode array detection. J Chromatogr A . 2008;1211(1-2):22-32.
Weber F-A, Aus Der Beek T, Bergmann A, Carius A, Grüttner G, Berlin G, et al. Pharmaceuticals in the environment-the global perspective Occurrence, effects, and potential cooperative action under the Strategic Approach to International Chemicals Management (SAICM) [Internet]. 2014. Available from: www.stoffers-steinicke.de
» www.stoffers-steinicke.de
Yilmaz B, Ciltas U. Determination of diclofenac in pharmaceutical preparations by voltammetry and gas chromatography methods. J Pharm Anal. 2015;5(3):153-160.
Zhao S, Bai W, Yuan H, Xiao D. Detection of paracetamol by capillary electrophoresis with chemiluminescence detection. Anal Chim Acta. 2006;559(2):195-199.
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