UPLC-MS/MS and Dushman reaction based spectrophotometric method for determination of Ceftazidime, an antibiotic, in medicinal formulation

SIDDIQUI, Masoom Raza; HAKAMI, Afnan Ali Hussain; WABAIDUR, Saikh Mohammad; ALOTHMAN, Zeid Abdullah; KHAN, Moonis Ali; HUSAIN, Fohad Mabood

doi:10.1590/fst.07020

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Original Article • Food Sci. Technol (Campinas) 41 (1) • Jan-Mar 2021 • https://doi.org/10.1590/fst.07020 linkcopy

UPLC-MS/MS and Dushman reaction based spectrophotometric method for determination of Ceftazidime, an antibiotic, in medicinal formulation

Authorship SCIMAGO INSTITUTIONS RANKINGS

Two analytical methods were developed, one utilizing sensitive UPLC-MS/MS method while other being the spectrophotometric method exploiting the Dushman reaction. Both methods were validated based on ICH guidelines and were successfully applied to quantitate the drug in marketed formulation. UPLC-MS/MS method responded linearly in the range of 1.6 µgmL^-1-6.4 µgmL^-1 while spectrophotometric procedure followed the Beer’s law in the concentration range of 30-100 µgmL^-1. UPLC-MS/MS has been found to have a limit of quantitation of 0.97 µgmL^-1 while spectrophotometric method was found to quantitate 14.00 µgmL^-1 correctly with high precision. Both the methods showed an excellent recovery of 99.36%-100.91% (% RSD 1.05-1.73) and 98.64%-99.73% (%RSD 0.67-1.68) for UPLC-MS/MS and spectrophotometric, respectively.

Keywords:
Ceftazidime; UPLC-MS/MS; method development; spectrophotometry

Analytical Parameters	Spectrophotometry	UPLC-MS/MS
λ_max / Ionization mode	352	Positive
Linear dynamic range	30-100	1.6-6.4
Linear regression equation	A = -0.1554+0.0157*C	A = -155.65 + 330.56 *C
S₀*	0.0220	29.27
Intercept (a)	-0.1554	-155.65
Slope (b)	0.0157	330.56
Correlation coefficient (r)	0.9986	0.9989
Detection limit	4.62	0.32
Quantitation limit	14.0	0.969

Precision	Theoretical	Spectrophotometry			LC-MS/MS
Precision	Theoretical	30	60	90	2.4	4.8	6.4
Intra-day	Nominal ± SD	29.81 ± 0.42	59.74 ± 0.39	89.88 ± 0.65	2.39 ± 0.02	4.76 ± 0.07	6.40 ± 0.09
Intra-day	Recovery ± RSD	99.35 ± 1.40	99.57 ± 0.65	99.86 ± 0.73	99.94 ± 0.91	99.20 ± 0.03	100.02 ± 1.42
Inter-day	Nominal ± SD	29.69 ± 0.52	59.98 ± 0.46	89.96 ± 0.99	2.41 ± 0.04	4.81 ± 0.07	6.39 ± 0.12
Inter-day	Recovery ± RSD	98.96 ± 1.74	99.97 ± 0.77	99.96 ± 1.09	100.34 ± 1.79	100.23 ± 1.62	99.92 ± 1.92

Formulation	Spectrophotometry					LC-MS/MS
Formulation	Theoretical	Spiked	Nominal	RSD	Recovery	Theoretical	Spiked	Nominal	RSD	Recovery
Bectozid 1gm	30	30	59.19	0.80	98.64	1.6	1.6	3.18	1.05	99.36
	30	40	69.81	0.67	99.73	1.6	2.4	4.00	1.73	100.09
	30	50	79.74	1.68	99.67	1.6	3.2	4.78	1.21	99.50
	30	70	98.91	1.33	98.91	1.6	4.8	6.46	1.40	100.91

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[TFN1] ^*
S₀ – Standard deviation of the calibration curve.