An innovative, simple, fast, and less toxic high-performance liquid chromatographic method for determination of prednisone in capsules

Silva, Pedro Henrique Reis da; Enéas, Paula Cristina Rezende; Fernandes, Christian; Pianetti, Gerson Antônio

doi:10.1590/s2175-97902017000216064

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Brazilian Journal of Pharmaceutical Sciences

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Article • Braz. J. Pharm. Sci. 53 (2) • 2017 • https://doi.org/10.1590/s2175-97902017000216064 copy

An innovative, simple, fast, and less toxic high-performance liquid chromatographic method for determination of prednisone in capsules

Authorship SCIMAGO INSTITUTIONS RANKINGS

ABSTRACT

Prednisone is an anti-inflammatory steroid drug widely used in clinical practice. However, no high-performance liquid chromatographic (HPLC) method has been described in the literature for the determination of prednisone in capsules until now. Thus, an HPLC method was developed using a C18 (250x4.0, 5 µm) column, with methanol:water (70:30) as mobile phase at a flow rate of 1 mL/min and detection at 240 nm. The developed method was validated following current Brazilian legislation. Additionally, linearity was assessed by evaluating the assumptions of normality, homoscedasticity, and independency of residuals, and the fit to the linear model. The method showed linearity (r²>0.99) over the range of 14.0-26.0 µg/mL, selectivity, precision (RSD<2.0%), robustness, and accuracy (average recovery of 100.05%). The chromatographic procedure was applied for assay and uniformity content determination of three different batches of prednisone capsules, showing to be suitable for their quality control.

Uniterms:
Prednisone; Capsules; High performance liquid chromatography/validation; Linearity assessment.

Excipients	Batches (%)			Role
Excipients	A	B	C
Colloidal silicon dioxide	0.5	1.0	4.2	Glidant
Sodium lauryl sulfate	1.5	-	-	Tensoactive
Magnesium stearate	0.5	-	-	Lubricant
Lactose monohydrate M200	82.5	-	79.1	Diluent
Polyvinylpyrrolidone (Kollidon K30)	15.0	-	16.7	Binder
Corn starch	-	67.5	-	Diluent
Talc	-	30.5	-	Glidant

Parameters	Nominal	1	2	3	4	5	6
Ratio of methanol (%)	70	67	73	70	70	70	70
Mobile phase flow-rate (mL/min)	1	1	1	1	1	0.8	1.2
Temperature (°C)	25	25	25	20	30	25	25

Regression parameters	Results
Coefficient of determination (^_r2 )	0.9961
Slope ± standard deviation	44.912 ± 0.646
Intercept ± standard deviation	6.535 ± 13.172
Range (%)	70 - 130
Number of points	7

Unit	Batch (%)
Unit	A	B	C
1	97.57	93.41	89.35
2	98.53	92.90	88.01
3	98.00	94.13	90.94
4	97.41	92.12	88.25
5	99.60	91.57	88.20
6	100.09	91.07	88.21
7	98.62	91.31	88.08
8	100.37	92.69	89.27
9	99.53	92.53	90.78
10	98.31	91.53	88.80
Mean	98.80	92.33	88.99
Standard deviation	1.04	0.99	1.09
RSD (%)	1.05	1.07	1.23
Acceptance value	2.52	8.74	12.46

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: P.H.R. Silva. Faculdade de Farmácia. Universidade Federal de Minas Gerais - 31270-901- Belo Horizonte, MG, Brasil. Phone: + 55-31-34096957. Fax: +55-31-34096976. E-mail: ordepreis_minas@hotmail.com

Replicate	Content (%)
Replicate	Day 1	Day 2
1	98.31	99.97
2	100.39	99.28
3	100.86	98.74
4	98.96	98.16
5	99.68	98.50
6	100.27	99.48
Mean	99.75	99.02
RSD (%)	0.96	0.68

Batch	Level (%)	Recovery (%)
A	80	100.61
	100	99.94
	120	100.79
B	80	99.19
	100	99.77
	120	99.56
C	80	100.51
	100	99.73
	120	100.32
Mean		99.38
RSD (%)		0.88

Replicate	Content (%)
Replicate	Batch A	Batch B	Batch C
1	98.65	93.51	89.63
2	98.88	92.92	90.32
3	98.32	92.61	90.25
Mean	98.62	93.01	90.07
RSD (%)	0.28	0.43	0.42