Solid Phase Extraction and Simultaneous Chromatographic Quantification of some Non-steroidal Anti-inflammatory Drug Residues; an Application in Pharmaceutical Industrial Wastewater Effluent

Korashy, Mohamed A. R.; Gawad, Sherif A. Abdel; Hassan, Nagiba Y.; AbdelKawy, M.

doi:10.1590/s2175-97902022e18691

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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/s2175-97902022e18691 copy

Solid Phase Extraction and Simultaneous Chromatographic Quantification of some Non-steroidal Anti-inflammatory Drug Residues; an Application in Pharmaceutical Industrial Wastewater Effluent

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

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.

Keywords:
Non-steroidal anti-inflammatory drugs; HPLC; Wastewater; TLC; SPE

		HPLC				TLC			Reference Value
	PCM	DCF	IBP	IND	PCM	DCF	IBP	IND	Reference Value
Resolution (R)*	-	4.58	5.83	136.76	-	1.26	1.30	3.00	R > 1.25
Tailing Factor (T)	0.99	0.95	0.98	0.96	-	-	-	-	T=1 for a typical symmetric peak
Capacity factor (k)**	0.68	6.52	6.81	6.31	0.18	0.56	0.69	0.44	1-10 acceptable for HPLC
Capacity factor (k)**	0.68	6.52	6.81	6.31	0.18	0.56	0.69	0.44	0-1 acceptable for TLC
Selectivity (α) ***	-	1.03	1.04	9.34	-	3.11	3.83	2.44	> 1
Column efficiency (N)****	36097.19	416734.69	356003.92	384909.88	-	-	-	-	Increases with efficiency of the separation
Height Equivalent to theoretical Plates (HETP)	6.93×10^-4	6.00×10^-5	7.02×10^-5	6.50×10^-5	-	-	-	-	The smaller the value, the higher the column efficiency
Symmetry Factor					1.00	0.95	0.98	1.00

Parameter			HPLC				TLC
Parameter		PCM	DCF	IBP	IND	PCM	DCF	IBP	IND
Slope*		103.4	218.4	425.7	219.9	5963	8420	1971	9683
Intercept		9.856	24.02	45.01	27.43	819.6	673.8	1401	-837.5
Range**		0.25-15	0.2-15	0.25-15	0.25-15	0.1-0.9	0.1-0.9	1.0-9.0	0.1-0.9
Correlation coefficient (r)		0.999	0.999	0.999	0.999	0.999	0.998	0.999	0.999
Specificity (mean±SD)		99.54± 0.84	99.34± 0.64	99.26± 1.36	99.96± 1.37	99.56± 0.55	100.33± 1.93	99.53± 1.36	99.05± 0.45
Accuracy (mean±SD)		100.02± 0.86	99.77± 0.99	99.77± 1.09	99.58± 0.61	99.67± 1.72	99.76± 1.78	99.73± 0.83	99.2± 1.62
Precision	Intraday ****	0.19	0.41	0.13	0.14	0.30	0.13	0.86	0.20
(% RSD)***	Interday*****	1.01	0.75	0.42	0.13	1.01	0.51	0.54	0.95
LOD* (μg/mL)		6.38×10^-3	1.51×10^-3	1.18×10^-3	2.29×10^-3	3×10^-4	7.58×10^-4	2.2×10^-3	4×10^-4
LOQ* (μg/mL)		1.93×10^-2	4.57×10^-3	3.58×10^-3	6.94×10^-3	9.2×10^-4	2.29×10^-3	6.9×10^-3	1.22×10^-3

Item	Official method*				HPLC				TLC
	PCM	DCF	IBP	IND	PCM	DCF	IBP	IND	PCM	DCF	IBP	IND
Mean	99.92	99.92	99.82	99.5	99.54	99.34	99.26	99.96	99.56	99.53	100.33	99.05
SD	0.37	0.37	0.54	0.58	0.84	0.64	1.36	1.37	0.55	1.36	1.93	0.45
Variance	0.14	0.14	0.29	0.34	0.7	0.41	1.86	1.87	0.3	1.84	3.72	0.2
N	5	5	5	5	5	5	5	5	5	5	5	5
Student’s t-test (2.306)**	-	-	-	-	0.93	1.75	0.85	0.69	1.22	0.62	0.57	1.37
F value (6.3882)**	-	-	-	-	5.11	2.99	6.38	5.56	2.19	13.44	12.76	1.68

Results of One Way Repeated Anova							Comparison Between Techniques*
Source of variation		Sum of Squares	df	Mean Square	F	Sig.	(I) Techniques	(J) Techniques	Mean Difference (I-J)	Sig.^a
PCM	Between Techniques	16.06	1.00	16.06	2.28	0.17	1.00	2.00	1.89	0.17
PCM	Error(Between Samples	418.00	8.00	52.25			1.00	2.00	1.89	0.17
DCF	Between Techniques	1.39	1.00	1.39	0.43	0.53	1.00	2.00	0.56	0.53
DCF	Error(Between Samples	179.44	8.00	22.43			1.00	2.00	0.56	0.53
IBP**	Between Techniques	-	-	-	-	-	-	-	-	-
IBP**	Error(Between Samples	-	-	-			-	-	-	-
IND	Between Techniques	18.00	1.00	18.00	3.27	0.11	1.00	2.00	2.00	0.11
IND	Error(Between Samples	1037.78	8.00	129.72			1.00	2.00	2.00	0.11

		HPLC				TLC
	PCM	DCF	IBP	IND	PCM	DCF	IBP	IND
Sample1	3.9	-	-	1.5	3.64	-	-	1.73
Sample2	-	3.4	2.9	-	-	3.1	-	-
Sample3	2.8	3.1	-	-	2.75	3.3	-	-
Sample4	3.5	-	1.25	-	3.8	-	-	-
Sample5	-	-	-	1.4	-	-	-	1.65

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: M. A.R. Korashy. Mobile: +2 01093556454. Email: Mohamed_korashy2007@yahoo.com. List of authors: Sherif A. Abdel Gawad: sagawad@yahoo.com 0112366633. Nagiba Yehia Hassan: nagiba.hassan@pharma.cu.edu.eg 01111859054. M. AbdelKawy: dr.mohabdelkawy@ hotmail.com 01005002155