Simultaneous determination of paracetamol, dextromethorphan, chlorpheniramine, pseudoephedrine and major impurities of paracetamol and pseudoephedrine by using capillary electrophoresis

Yener, Beytul; Erkmen, Cem; Uslu, Bengi; Goger, Nilgun Gunden

doi:10.1590/s2175-97902022e19836

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Brazilian Journal of Pharmaceutical Sciences

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Article • Braz. J. Pharm. Sci. 58 • 2022 • https://doi.org/10.1590/s2175-97902022e19836 copy

Simultaneous determination of paracetamol, dextromethorphan, chlorpheniramine, pseudoephedrine and major impurities of paracetamol and pseudoephedrine by using capillary electrophoresis

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

A capillary electrophoresis method was developed for the first time and optimized for the determination of paracetamol, pseudoephedrine, dextromethorphan, chlorpheniramine, 4-aminophenol and ephedrine in tablet formulation. Optimum electrophoretic conditions were achieved by using a background electrolyte of 75 mmol L^-1 sodium borate buffer at pH 8.0, a capillary temperature of 30°C, a separation voltage of 30 kV and a pressure injection of the sample at 50 mbar for 10 s. Calibration graphs showed a good linearity with a coefficient of determination (R²) of at least 0.999 for all compounds. Intraday and interday precision (expressed as relative standard deviation (RSD) %) were lower than 1.39% for capillary electrophoresis method. The developed method was demonstrated to be simple and rapid for the determination of paracetamol, pseudoephedrine, dextromethorphan, chlorpheniramine, 4-aminophenol and ephedrine in tablet formulation providing recoveries in the range between 99.62 and 100.57% for all analytes.

Keywords:
Capillary electrophoresis; Chlorpheniramine; Dextromethorphan; Paracetamol; Pseudoephedrine

Parameters	DEX	EPH	CHL	PSE	4-AP	PAR
Average migration time (min)	5.83±0.03	6.05±0.08	6.53±0.05	7.21±0.01	9.23±0.05	10.79±0.08
Number of theoretical plates (N; plate/ meter )	9886	10164	11642	8766	9884	12692
Asymmetry factor	0.98	1.01	0.97	1.02	1.07	1.03
Average peak area	143.92±0.79	89.32±0.34	71.55±0.92	634.64±1.44	103.65±0.44	3436.60±6.38
Capacity factor	3.85	4.04	4.43	5.01	6.69	8.04
Resolution (Rs)	-	3.44	3.21	5.22	10.2	8.75
Selectivity (α)	-	1.05	1.10	1.14	1.33	1.21

BGE solution	75 mM sodium borate (pH: 8.0)
Organic solvent	15%- Acetonitrile
Wavelength	192 nm
Applied voltage	30 kV
Capillary temperature	30 °C
Sample pH	7.0
Injection time	10.0 s
Diameter of capillary	75 μm

Regression parameters	PAR	4-AP	PSE	CHL	EPH	DEX
Regression equation	$y = 4.22 x + 3.45$	$y = 6.94 x - 0.73$	$y = 8.58 x - 8.64$	$y = 15.03 x - 3.93$	$y = 6.01 x - 0.23$	$y = 3.66 x + 7.21$
Determination coefficient (R ² )	0.9996	0.999	0.9997	0.9995	0.9996	0.9991
Calibration range (μg mL ^-1 )	50-900	5-20	25-120	2-10	5-20	25-100
LOD (μg mL ^-1 )	12.40	1.00	5.10	0.40	1.10	4.50
LOQ (μg mL ^-1 )	37.50	2.90	15.60	1.20	3.40	13.60
Repeatability intra-day (RSD% n=3)	0.04	0.47	0.08	1.39	0.7	0.16
Repeatability inter-day (RSD% n=3)	0.17	0.63	0.11	1.31	1.01	0.49

Parameters	Quantifications results						Recovery results
Parameters	PAR	4-AP	PSE	CHL	EPH	DEX	PAR	4-AP	PSE	CHL	EPH	DEX
Claimed amount (mg tablet ^-1 )	325.00	6.00	30.00	2.00	6.00	15.00	100.00	100.00	100.00	100.00	100.00	100.00
*Found amount (mg tablet** ^-1 )	325.16	5.99	29.77	2.02	5.99	14.82	99.92	99.76	99.62	100.57	100.10	100.14
Bias (%)	0.83	0.019	0.74	0.13	0.05	0.82	1.38	1.09	1.49	1.40	1.15	1.91
*RDS (%)**	0.09	0.31	0.09	0.09	0.83	0.09	1.49	1.09	1.49	1.39	1.14	1.90

Analyte	Method	Calibration range (μg mL^-1)	LOD (μg mL^-1)	LOQ (μg mL^-1)	Retention Time or Migration Time (min)	Recovery (%)	Application	Reference
PAR	LC	4-240.00	0.10	0.29	4.19	99.80	Sugar coated tablet formulation	(Palabiyik, Onur, 2007Palabiyik İM, Onur F. The Simultaneous determination of phenylephrine hydrochloride, paracetamol, chlorpheniramine maleate and dextromethorphan hydrobromide in pharmaceutical preparations. Chromatographia. 2007;66:93-96. doi: 10.1365/s10337-007-0324-5. https://doi.org/10.1365/s10337-007-0324-... )
DEX		0.40-19.00	0.13	0.38	7.04	99.90
CHL		0.48-44.00	0.08	0.24	6.39	99.10
PAR	CE	50.00-600.00	12.34	50.00	5.13	99.90-101.62	Sugar coated tablet formulation	(Palabiyik, Onur, 2010Palabiyik İM, Onur F. Multivariate optimization and validation of a capillary electrophoresis method for the simultaneous determination of dextromethorphan hydrobromur, phenylephrine hydrochloride, paracetamol and chlorpheniramine maleate in a pharmaceutical preparation using response surface methodology. Anal Sci. 2010;26(8):853-859. doi: 10.2116/analsci.26.853. https://doi.org/10.2116/analsci.26.853... )
DEX		4.00-20.00	1.94	4.00	3.31	100.21-102.10
CHL		1.60-8.00	0.007	1.60	3.51	99.55-101.62
PSE	CE	8.00-520.00	1.94	-	~ 3.90	92.00-98.00	Tablet formulations	(*Dong et al., 2005*Dong Y, Chen X, Chen Y, Chen X, Hu Z. Separation and determination of pseudoephedrine, dextromethorphan, diphenhydramine and chlorpheniramine in cold medicines by nonaqueous capillary electrophoresis. J Pharm Biomed Anal . 2005;39(1-2):285-289. doi:10.1016/j.jpba.2005.02.032. https://doi.org/10.1016/j.jpba.2005.02.0... )
DEX		2.50-160.00	0.98	-	~ 5.00	91.00-109.00
CHL		4.50-300.00	1.19	-	~ 6.50	91.00-105.00
PAR	Normal-phase LC	250.00-750.00	-	-	~ 1.50	99.20	Tablet formulation	(Al-Rimawi, 2010Al-Rimawi F. Normal-phase LC method for simultaneous analysis of pseudophedrine hydrochloride, dextromethorphan hydrobromide, chlorpheniramine maleate, and paracetamol in tablet formulations. Saudi Pharm J. 2010;18(2):103-106. doi:10.1016/j.jsps.2010.02.006. https://doi.org/10.1016/j.jsps.2010.02.0... )
PSE		150.00-450.00	-	-	~ 3.50	99.70
CHL		10.00-30.00	-	-	~ 7.00	98.10
DEX		75.00-225.00	-	-	~ 5.50	98.60
PAR	CE	50.00-900.00	12.40	37.50	5.83	99.92	Tablet formulation	This study
4-AP		5.00-20.00	1.00	2.90	9.23	99.76
PSE		25.00-120.00	5.10	15.60	7.21	99.62
CHL		2.00-10.00	0.40	1.20	6.53	100.57
EPH		5.00-20.00	1.10	3.40	6.05	100.10
DEX		25.00-100.00	4.50	13.60	10.79	100.14

Universidade de São Paulo, Faculdade de Ciências Farmacêuticas Av. Prof. Lineu Prestes, n. 580, 05508-000 S. Paulo/SP Brasil, Tel.: (55 11) 3091-3824 - São Paulo - SP - Brazil
E-mail: bjps@usp.br

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[1] *Correspondence: N. G. Goger. Gazi University. Faculty of Pharmacy. Department of Analytical Chemistry. 06330, Ankara, Turkey. Phone: +90 3122023104. Fax: +90 312 4333419. E-mail: ngoger@gazi.edu.tr. ORCID iD: https://orcid.org/0000-0002-7376-9879.