Stability indicating RP-HPLC method for simultaneous determination of gatifloxacin and dexamethasone in binary combination

Razzaq, Syed Naeem; Ashfaq, Muhammad; Khan, Islam Ullah; Mariam, Irfana; Razzaq, Syed Saleem; Mustafa, Ghulam; Zubair, Muhammad

doi:10.1590/s2175-97902017000115177

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Brazilian Journal of Pharmaceutical Sciences

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Article • Braz. J. Pharm. Sci. 53 (1) • 2017 • https://doi.org/10.1590/s2175-97902017000115177 copy

Stability indicating RP-HPLC method for simultaneous determination of gatifloxacin and dexamethasone in binary combination

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

In this study, conditions were optimized for development of a simple RP-HPLC method for simultaneous analysis of gatifloxacin and dexamethasone in different matrices like pharmaceuticals, human serum and urine. Good separation of gatifloxacin and dexamethasone from the induced degradation products was accomplished using C8 as stationary phase; 0.02 M phosphate buffer (pH 3.0) and methanol (42:58 v/v) as mobile phase. The concentration was measured with DAD at 270 nm. Linearity was observed in the range of 0.000040-0.000280 mol/L for gatifloxacin (r²≥0.999) and 0.000013-0.000091 mol/L for dexamethasone (r²≥0.999). Both the analyte peaks were completely separated from the peaks of induced degradation products as indicated by the peak purity index (≥0.9999 for both analytes). The optimized method is recommended to be used for concurrent analysis of gatifloxacin and dexamethasone in different matrices.

Uniterms:
Gatifloxacin; Dexamethasone; High performance liquid chromatography; Validation; Plasma; Degradation products.

Nature of Sample	Spiked Concentrations mol/L	Measured Concentration mol/L ± RSD (%)	Recovery (%)
Pharmaceutical Formulations			Recovery (%)
Gatifloxacin	0.000080	0.0000806 ± 1.19	100.7
	0.000160	0.000160 ± 0.41	100.0
	0.000240	0.0002431 ± 0.91	101.3
Dexamethasone	0.000026	0.0000259 ± 0.49	99.50
	0.000052	0.0000523 ± 1.24	100.5
	0.000078	0.0000785 ± 0.61	100.7
Spiked Serum			100.7
Gatifloxacin	0.000080	0.000072 ± 1.65	90.0
	0.000160	0.000147 ± 3.24	91.9
	0.000240	0.000219 ± 1.33	91.4
Dexamethasone	0.000026	0.0000258 ± 1.39	99.2
	0.000052	0.0000525 ± 1.93	100.9
	0.000078	0.000079 ± 1.90	101.3
Spiked Urine			101.3
Gatifloxacin	0.000080	0.0000796 ± 1.14	99.5
	0.000160	0.000163 ± 0.68	101.8
	0.000240	0.000244 ± 1.79	101.5
Dexamethasone	0.000026	0.0000261 ± 1.94	100.2
	0.000052	0.0000523 ± 1.61	100.5
	0.000078	0.0000782 ± 1.31	100.3

Drugs	Actual Concentration mol/L	Intra-Day Precision Measured Concentration mol/L ± RSD (%)	Inter-Day precision Measured Concentration mol/L ± RSD (%)
Pharmaceutical Formulations
Gatifloxacin	0.000080	0.0000783 ± 1.21	0.0000803 ± 1.87
	0.000160	0.0001614 ± 1.92	0.0001627 ± 0.99
	0.000240	0.0002400 ± 0.81	0.0002406 ± 0.82
Dexamethasone	0.000026	0.0000262 ± 1.87	0.0000260 ± 1.41
	0.000052	0.0000525 ± 0.51	0.0000526 ± 1.89
	0.000078	0.0000780 ± 1.22	0.0000777 ± 1.20
Spiked Serum
Gatifloxacin	0.000080	0.0000767 ± 1.58	0.0000758 ± 2.26
	0.000160	0.0001471 ± 2.99	0.0001511 ± 2.94
	0.000240	0.0002252 ± 1.10	0.0002205 ± 2.09
Dexamethasone	0.000026	0.0000260 ± 1.15	0.0000261 ± 2.14
	0.000052	0.0000526 ± 2.17	0.0000520 ± 2.43
	0.000078	0.0000780 ± 1.95	0.0000782 ± 1.18
Spiked Urine
Gatifloxacin	0.000080	0.0000797 ± 1.54	0.0000804 ± 2.16
	0.000160	0.0001623 ± 1.08	0.0001647 ± 1.04
	0.000240	0.0002402 ± 1.54	0.0002406 ± 1.72
Dexamethasone	0.000026	0.0000262 ± 1.08	0.0000262 ± 1.54
	0.000052	0.0000523 ± 1.53	0.0000525 ± 1.13
	0.000078	0.0000781 ± 1.29	0.0000776 ± 1.34

Chromatographic conditions	Assay (%)	t_R (min)	Plates	Tailing
Methanol: buffer (61:39)	98.7	2.99	4507	1.42
Methanol: buffer (58:42)	100.6	3.38	4588	1.41
Methanol: buffer (55:45)	100.9	3.69	4478	1.44
Flow rate (1.3 mL/min)	100.9	3.75	4601	1.43
Flow rate (1.5 mL/min)	99.8	3.38	4577	1.43
Flow rate (1.7 mL/min)	100.5	2.89	4587	1.41
Buffer (pH 2.8)	102.0	3.34	4691	1.44
Buffer (pH 3.0)	101.5	3.38	4511	1.41
Buffer (pH 3.2)	99.6	3.38	4547	1.40

Chromatographic conditions	Assay (%)	t_R (min)	Plates	Tailing
Methanol: buffer (61:39)	101.7	7.52	6821	1.20
Methanol: buffer (58:42)	100.9	7.75	6799	1.21
Methanol: buffer (55:45)	100.0	7.92	6647	1.21
Flow rate (1.3 mL/min)	99.9	9.19	6788	1.20
Flow rate (1.5 mL/min)	99.9	7.75	6718	1.22
Flow rate (1.7 mL/min)	99.5	6.82	6895	1.23
Buffer (pH 2.8)	100.7	7.75	6805	1.22
Buffer (pH 3.0)	98.7	7.77	6705	1.24
Buffer (pH 3.2)	100.7	7.74	6611	1.22

Nature of stress	Storage condition (°C/%RH)	Time (h)	Amount of gatifloxacin remaining ± RSD (%)	Amount of dexamethasone remaining ± RSD (%)	Extent of decomposition
5 M HCl	(40/75)	1	100.1 ± 1.2	101.3 ± 0.30	None
	(40 /75)	8	99.7 ± 1.0	97.6 ± 1.1	None
	(40/75)	16	97.2 ± 0.80	90.0 ± 1.5	Slight
	(40/75)	23	100.3 ± 0.90	68.6 ± 1.2	Substantial
5 M NaOH	(40/75)	16	93.7 ± 1.7	4.8 ± 2.3	Substantial
6% H2O2	(40/75)	1	98.6 ± 1.5	100.8 ± 1.5	None
	(40/75 )	8	101.2 ± 1.4	100.5 ± 1.4	None
	(40/75)	23	95.5 ± 1.4	100.6 ± 1.5	None
	(40/75	70	96.8 ± 1.1	96.7 ± 1.9	None
Thermal	(40/75 )	1	100.3 ± 0.80	99.5 ± 1.5	None
	(40/75)	16	99.7 ± 0.40	100.4 ± 1.4	None
	(40/75)	24	100.0 ± 1.3	102.8 ± 1.5	None
	(40/75 )	70	98.5 ± 1.0	93.2 ± 1.7	None
Photolytic	Sunlight	2	99.8 ± 1.9	102.9 ± 1.2	None
	Sunlight	4	98.6 ± 1.4	102.3 ± 1.4	None
	Sunlight	6	91.3 ± 1.9	78.4 ± 1.4	Substantial

Product	Ingredient	Label value (mg/mL)	Recovery (%) ± RSD (%)
GATE DX	gatifloxacin	3	100.3 ± 0.30
GATE DX	dexamethasone	1	99.00 ± 0.70
GATIBLU-D	gatifloxacin	3	100.7 ± 0.10
GATIBLU-D	dexamethasone	1	98.90 ± 0.70

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. Ashfaq. Department of Chemistry. University of Gujrat. 50700, Gujrat,Pakistan. E-mail: ashfaqchemist@hotmail.com. I.U. Khan. Department of Chemistry. Government College University. 54000, Lahore Pakistan. Email: iukhan@gcu.edu.pk