Development and validation of UV-spectrophotometric methods for the determination of sumatriptan succinate in bulk and pharmaceutical dosage form and its degradation behavior under varied stress conditions

Peer review under responsibility of University of Bahrain.

Figures & data

Figure 1 Structure of sumatriptan succinate.

Table 1 Comparison of the proposed and the existing visible spectrophotometric methods.

Sl. No.	Reagent/s	λmax, nm	Beer’s law range, μg mL^−1 (ε in l mol^−1 cm^−1)	Remarks	Ref.
1	Bromate–bromide-			Multi step reaction, time consuming	Satyanarayana and Nageswara Rao (2011)
	(a) methyl orange,	508	0.2–1.6 (1.90 × 10^5)
	(b) indigo carmine	610	2.0–12.0 (2.71 × 10^4)
2	Folin-Ciocaltaeu reagent	760	2.0–6.0	Multi step reaction	Tipre and Vavia (1999)
3	Sodium nitroprusside acetaldehyde	552	4.0–20.0 (1.10 × 10^4)	Requires rigid pH control	Kalyanaramu and Raghubabu (2011b)
4	(a) Brucine–sodium metaperiodate,	520	4.0–20.0	Multi step reaction	Kalyanaramu and Raghubabu (2011d)
	(b) citric acid-acetic anhydride	580	8.0–24.0
5	Folin reagent	455.6	16.0–48.0 (3.85 × 10^3)	Strict pH control, time consuming.	Kalyanaramu and Raghubabu (2010)
6	Cobalt thiocyanate	629.4	16.0–48.0 (3.97 × 10^3)	Involves extraction step	Kalyanaramu and Raghubabu (2011a)
7	Tropaeolin-OOO	482.5	2.0–10.0 (2.08 × 10^4)	Requires rigid pH control; involves liquid–liquid extraction	Kalyanaramu and Raghubabu (2011c)
8	p-Chloranilic acid	520	20.0–184.0 (9.28 × 10^2)	Less sensitive	Fathima et al. (2012)
9	UV-absorption measured in water.	220	1.0–12.0	No stress studies	Prabahar et al. (2009)
10	UV-absorption measured in water.	282	21.0–39.0	No stress studies	Pourmand et al. (2011)
11	UV-absorption measured in			Stress studies were performed, highly sensitive.	Proposed methods
	(a) 0.1 M HCl	226	7.59 × 10^4
	(b) acetonitrile	228	7.81 × 10^4

Figure 2 Absorption spectra of STS in 0.1 M HCl (method A) and in acetonitrile (method B).

Table 2 Regression and analytical parameters.

Parameter	Method A	Method B
λmax, nm	226	228
Beer’s law limits (μg ml^−1)	0.2–6.0	0.2–6.0
Molar absorptivity (l mol^−1 cm^−1)	7.59 × 10^4	7.81 × 10^4
Sandell sensitivity^⁎ (μg cm^−2)	0.0054	0.0047
Limit of detection (μg ml^−1)	0.05	0.05
Limit of quantification (μg ml^−1)	0.14	0.16
Regression equation, Y^⁎⁎
Intercept, (a)	0.0014	−0.0252
Slope, (B)	0.1807	0.2108
Correlation coefficient (r)	0.9999	0.9999
Standard deviation of intercept (Sa)	0.0165	0.0444
Standard deviation of slope (Sb)	0.0048	0.0178

⁎ Limit of determination as the weight in μg per ml of solution, which corresponds to an absorbance of A = 0.001 measured in a cuvette of cross-sectional area 1 cm² and l = 1 cm.

⁎⁎ Y = a + bX, where Y is the absorbance, a is the intercept, b is the slope and X is the concentration in μg ml⁻¹.

Table 3 Evaluation of intra-day and inter-day precision and accuracy.

Method	STS taken (μg ml^−1)	Intra-day (n = 7)			Inter-day (n = 5)
		STS found^a (μg ml^−1)	% RSD^b	% RE^c	STS found^a (μg ml^−1)	% RSD^b	% RE^c
Method A	1.00	1.01	0.60	0.99	1.02	0.90	1.73
	3.00	2.98	1.26	0.52	2.97	1.21	0.91
	5.00	5.06	0.71	1.13	5.07	1.08	1.37
Method B	1.00	1.02	0.91	1.98	1.03	1.10	2.62
	3.00	3.06	1.35	2.11	3.07	1.58	2.24
	5.00	4.97	1.04	0.52	5.06	0.71	1.16

a Mean value of five determinations.

b Relative standard deviation (%).

c Relative error (%).

Table 4 Results of analysis of synthetic mixture by the proposed methods.

Method A			Method B
Synthetic mixture μg ml^−1	Total found, μg ml^−1	STS recovered^∗, percent ± SD	Synthetic mixture μg ml^−1	Total found, μg ml^−1	STS recovered^∗, percent ± SD
1.00	1.01	101.4 ± 0.01	1.00	1.02	102.9 ± 0.01
3.00	2.95	98.45 ± 0.03	3.00	3.10	103.5 ± 0.03
5.00	5.10	102.1 ± 0.08	5.00	5.07	101.4 ± 0.14

Table 5 Robustness and ruggedness.

Method	STS taken, μg ml^−1	Method robustness	Method ruggedness
		wavelengths, nm^a RSD, % (n = 3)	Inter-analysts RSD, % (n = 3)	Inter- cuvettes RSD, % (n = 3)
Method A	1.00	0.98	1.55	1.37
	3.00	1.24	0.85	1.83
	5.00	1.31	1.49	1.56
Method B	1.00	1.42	0.99	1.06
	3.00	0.77	1.37	1.65
	5.00	1.13	1.63	1.44

a Wavelengths used were 225, 226 and 227 in method A and 227, 228 and 229 in method B.

Table 6 Results of analysis of tablets by the proposed methods.

Tablet brand name	Label claim mg/tablet	Found (percent of label claim ± SD)^a
		Reference method	Proposed methods
			Method A	Method B
Suminat-25	25	99.78 ± 0.89	99.21 ± 0.95	101.1 ± 1.27
			t = 0.98	t = 1.90
			F = 1.14	F = 2.04
Suminat-50	50	100.6 ± 1.01	101.4 ± 1.34	102.1 ± 1.56
			t = 1.01	t = 1.80
			F = 1.76	F = 2.40

a Mean value of five determinations.

Tabulated t-value at the 95% confidence level is 2.78.

Tabulated F-value at the 95% confidence level is 6.39.

Table 7 Results of recovery study by standard addition method.

Tablets Studied	Method A				Method B
	STS in tablets, μg ml^−1	Pure STS added, μg ml^−1	Total found, μg ml^−1	Pure STS recovered^∗, Percent ± SD	STS in tablets, μg ml^−1	Pure STS added, μg ml^−1	Total found, μg ml^−1	Pure STS recovered^∗, Percent ± SD
Suminat-25	1.49	0.75	2.26	102.7 ± 2.52	1.52	0.75	2.29	102.7 ± 1.56
	1.49	1.50	3.01	101.3 ± 1.42	1.52	1.50	3.01	99.33 ± 0.84
	1.49	2.25	3.77	101.3 ± 1.30	1.52	2.25	3.82	102.2 ± 1.66
Suminat-50	1.52	0.75	2.26	99.07 ± 0.82	1.53	0.75	2.29	101.3 ± 0.78
	1.52	1.50	3.00	98.67 ± 1.47	1.53	1.50	3.04	100.7 ± 1.49
	1.52	2.25	3.81	101.8 ± 1.08	1.53	2.25	3.82	101.8 ± 1.37

Mean value of three determinations.

Figure 3 Acidic degradation. (a) (method A), (b) (method B).

Figure 4 Basic degradation. (a) (method A), (b) (method B).

Figure 5 Thermal degradation (a) (method A), (b) (method B) Photo degradation (c) (method A), (d) (method B).

Figure 6 Peroxide degradation (a) (method A), (b) (method B).