Acta Pharm.

57 (2007) 333–342 Original research paper

10.2478/v10007-007-0026-4

A sensitive spectrophotometric method for the determination

of sulfonamides in pharmaceutical preparations

PADMARAJAIAH NAGARAJA1* A new, simple and sensitive spectrophotometric method

SHAILENDRA D. NAIK2
for the determination of some sulfonamide drugs has been
ASHWINEE KUMAR SHRESTHA1
ANANTHARAMAN SHIVAKUMAR1 developed. The method is based on the diazotization of
sulfacetamide, sulfadiazine, sulfaguanidine, sulfamerazine,
1Department of Studies in Chemistry sulfamethazine, sulfamethoxazole, and their coupling with
University of Mysore, Manasagangothri 8-hydroxyquinoline in alkaline media to yield red colo-
Mysore-570006, India ured products with absorption maxima at 500 nm. Beer’s
law is obeyed from 0.1–7.0 mg mL–1. The limits of quantifi-
2 Charak Pharma Pvt. Ltd., Silvassa cation and limits of detection were 0.11–0.18 and 0.03–0.05
U. T. of Dadra Nagar Haveli mg mL–1, respectively. Intraday precision (RSD 0.1– 0.5%)
Silvassa-396230, India and accuracy (recovery 97.3–100.8%) of the developed me-
thod were evaluated. No interference was observed from
common adjuvants. The method has been successfully ap-
plied to the assay of sulpha drug in pharmaceutical for-
mulations.
Keywords: sulfonamide drugs, diazotization, 8-hydroxy-
Accepted June 26, 2007 quinoline, spectrophotometry, pharmaceutical formulation

Sulfonamides, important analogues of p-amino benzoic acid (1), are used in the tre-
atment of urinary track infections, eye infections and as a prophylaxis of rheumatic fever
(2). Antibacterial sulfonamides act as competitive inhibitors of the enzyme dihydropte-
roate synthetase, DHPS, in bacteria. DHPS catalyses the conversion of PABA (p-amino-
benzoate) to dihydropteroate, a key step in folate synthesis, which is necessary for the
cell to synthesize nucleic acids and thus exhibit a bacteriostatic effect (3).
Survey of the literature reveals various methods available for the determination of
sulfonamide derivatives. The methods include the nitrite method (4), GC (5), HPLC (6,
7), HPTLC (8), electroanalytical methods (9–12), immune chemical assay (13, 14), spec-
trofluorimetry (15), differential scanning calorimetry (16), surface enhanced Raman spec-
trometry (17), spectrophotometry (18–22). Most spectrophotometric methods suffer from
low sensitivity, high detection limits, tedious experimental conditions and complex pro-
cedures for the preparation of samples or standard solutions.
In the present study, we succeeded in developing a novel coupling agent for sensi-
tive and selective spectrophotometric determination of the sulfonamide class of drugs

* Correspondence, e-mail: [email protected]

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P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

based on the coupling of their diazotized form with 8-hydroxyquinoline (8-HQ), which
results in the formation of red coloured products in alkaline medium.

EXPERIMENTAL

Apparatus
A CHEMITO Model 2100 UV-VIS Spectrophotometer (Chemito Technologies Pvt Ltd.,
India) with 1-cm matched cells was used for all spectral and absorbance measurements.

Reagents
All the reagents and solvents were of analytical grade. The drugs selected for study
were procured from Charak Pharma Pvt. Ltd. (India), and their structures are given in
Table I: sulfacetamide (SFA, 99.0%, Sigma Spain), sulfamethazine (SFMt, 99.0%, Sigma
China), sulfadiazine (SFD, 99.0%, Sigma China) sulfaguanidine (SFG, 99.0%, Sigma Swit-
zerland), sulfamerazine (SFMr, 99.0%, Sigma Belgium), sulfamethoxazole (SFMx, 99.0%,
Sigma Belgium).

Table I. Sulfonamide drugs studied

Drug (code) Structure

Sulfacetamide (SFA) H2N SO2NHCOCH3

N
Sulfadiazine (SFD) H2N SO2NH
N

Sulfaguanidine (SFG) H2N SO2NC(NH2)2

CH3
N
Sulfamerazine (SFMr) H2N SO2NH
N
CH3
N
Sulfamethazine (SFMt) H2N SO2NH
N
CH3

H2N SO2NH
Sulfamethoxazole (SFMx)
N
O CH3

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P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

Standard solution of sulfonamide (1000 mg mL–1) was prepared by dissolving 100

mg each sulfonamide in 2.0 mL of sulfuric acid (10 mol L–1), then diluting with water to
mark in a 100-mL volumetric flask. A working standard solution of each sulfonamide
containing 25 mg mL–1 was prepared by further dilution and was standardized by the
British Pharmacopoeia method (4) and the reported method (21). An 8-HQ solution (0.5%,
m/V), sodium nitrite (1.0%, m/V) sulphamic acid (2%, m/V), sodium hydroxide (5 mol
L–1) and sulphuric acid (10 mol L–1) were prepared in water.

General procedure
Aliquots of standard sulfonamide solutions (SFMx, SFD, SFA, SFMt, SFMr and SFG)
were transferred into 25-mL calibrated flasks followed by 1.0 mL sulphuric acid to each.
After cooling in an ice bath, 1.5 mL of sodium nitrite (1.0% m/V) was added under swirl-
ing. The solutions were allowed to stand for 5 min and then 2.5 mL of sulphamic acid
(2.0%, m/V) was added, swirled and allowed to stand for 5 min. Then 2.0 mL of 8-HQ
(0.5%, m/V) was added, along with 2.0 mL of sodium hydroxide (5 mol L–1). The solu-
tion was made up to the mark with ethanol (95%), mixed thoroughly and after 5 min the
absorbance was measured at 500 nm against a reagent blank, and the calibration graph
was constructed.
The limit of detection (LOD) and quantification (LOQ) were calculated according to
the current ICH guidelines (23) as 3.3 and 10 standard deviation of the blank (n = 6) re-
spectively, divided by the slope of the calculation curve.
The range of the error was calculated using the following mathematical relation (24):

± t SD
n

where t = 2.571 (95% confidence limit), n = number of replicate determinations.

Assay of commercial samples

Tablets. – The following tablet formulations were purchased from local commercial
sources and used for the analysis: Septran tablet (Burroughs Wellcome, India) each con-
taining 400 mg of SFMx, Sulphadiazine tablet (Rhone Poulenc, India) each containing
500 mg of SFD.
Twenty tablets were powdered and mixed thoroughly. An amount equivalent to 50
mg sulfonamide was then dissolved in 20 mL of sulphuric acid (1 mol L–1) and filtered.
The filtrate was made up to 100 mL and appropriate aliquots of the solution were treat-
ed as mentioned above in the general procedure.
Eye drops. – The following eye drop formulations were purchased from local sources
and used for the analysis: Albucid (Nicholos-Pharmal India Ltd., India) containing 10
mg SFA mL–1, Locula (East India Ltd., India) containing 10 mg SFA mL–1.
A volume of 5 mL of eye drops (equivalent to 50 mg of SFA) was diluted with 2 mL
of sulphuric acid (10 mol L–1) and made up to 100 mL with water. The general procedure
was then followed.

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P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

RESULTS AND DISCUSSION

Chemistry
Sulfa drugs could be readily diazotized in acidic medium and the diazonium cation
would then react with a molecule of 8-HQ by electrophilic substitution at position-4 of
the coupling agent. The proposed method involves diazotization of sulfonamide deriva-
tives followed by their coupling with 8-HQ to produce a red coloured azo product. Job’s
method of continuous variation for determining the composition of the product indi-
cated that the reactants and reagents reacted in the 1:1 ratio. The proposed mechanism
of reaction between 8-HQ and the sulfonamide drug is illustrated in Fig. 1. To ascertain
the absorption maxima for sulfonamide derivatives, specified amounts of sulfonamide
derivatives were taken and the coloured reaction products were developed as mention-
ed in the general procedure, and the absorption maxima were found to be 500 nm. Fig. 2
shows the absorption spectrum of SFMx as the model compound. The resultant coloured
product was found to be stable for about two days. The value of absorbance decreased
above 30 °C. Hence, room temperature was preferred for the experiments. An attempt to
increase the stability of the product beyond 48 hours failed.

NO2–
H2N SO2NHCOCH3

SFA OH

N2+ SO2NHCOCH3

diazotized SFA

O N N SO2NHCOCH3

coupled product

Fig 1. Scheme of the proposed reaction mechanism.

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P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

0.7
Diazotised SFMx + 8-HQ

0.6 Blank

0.5

0.4
Absorbance

0.3

0.2

0.1

0
400 450 500 550 600 650 700
Wavelength (nm)
Fig. 2. Absorption spectrum of the reaction product of sulfamethoxazole
(SFMx) with 8-HQ (lmax= 500 nm).

Validation
The intraday precision of the proposed method was examined by carrying out six
replicate determinations of sulfonamides (within Beer’s law range) by the proposed me-
thod. Table II summarizes the RSD values (0.1–0.5%) and the range of error (0.20–0.35 at
95% confidence limit). The LOD was found to be in the range of 0.03 to 0.05 mg mL–1 and
LOQ was in the range of 0.11 to 0.18 mg mL–1. The recovery ranged from 97.3 ± 2.5% to
100.8 ± 1.2% (n = 6) (Table III).
The most promising feature of the proposed method is the freedom from interfe-
rences with the excipients commonly used in the pharmaceutical preparation of sulfo-
namide derivatives. Under optimum conditions, the effects of excipients and diluents
such as talc, glucose, dextrose, lactose, etc., were investigated. An amount far in excess
of that used in the pharmaceutical preparation was added in half the limit of Beer’s law
and no effect due to these excipients was found under the proposed experimental condi-
tions. The recovery range was from 99.2 ± 0.2% to 100.8 ± 0.4% (n = 6). The results are
presented in Table IV.

Application of the proposed method

The applicability of the proposed method for the assay of different pharmaceutical
formulations containing SFMx, SFD and SFA was examined for tablet and eye drops and
the results were statistically compared with those obtained by the official method based
on electrochemical titration (4) with NaNO2 and the reported spectrophotometric me-
thod (21) based on the reaction of drug with acetylacetone-formaldehyde reagent. The
t-test and F-test were carried out, which showed that the proposed method and other es-
tablished methods are of comparable accuracy and precision. The results are summa-
rized in Table V.

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P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

Table II. Some analytical parametres for the spectrophotometric determination of sulfonamide derivatives

Parameter SFMx SFD SFA SFMt SFMr SFG

Colour Red Red Red Red Red Red
ëmax (nm) 500 500 500 500 500 500
Stability (h) 48 48 42 48 46 48
Beer’s law range (mg mL–1) 0.2–6.0 0.1–5.0 0.2–6.0 0.3–7.0 0.1–4.0 0.19–6.0
Limit of detection (mg mL–1) 0.04 0.05 0.04 0.04 0.03 0.03
Limit of quantitation (mg mL–1) 0.15 0.16 0.15 0.18 0.12 0.11
Molar absorptivity (L mol–1 cm–1) 3.38 x 104 3.7 x 104 2.81 x 104 3.48 x 104 3.8 x 104 3.7 x 104

Regression equation (y)a

Slope (a) 0.143 0.145 0.124 0.130 0.136 0.125
Intercept (b) 0.011 0.005 0.007 0.004 0.003 0.012
Correlation coefficient (R) 0.9960 0.9984 0.9994 0.9980 0.9990 0.9992
RSD (%) 0.2 0.1 0.3 0.5 0.2 0.3
Range of error 0.3 0.2 0.4 0.3 0.2 0.3
(95% confidencee level) (%)
a y = a ã + b where ã is the concentration in mg mL–1.

Table III. Intraday accuracy and precision of the proposed method for SFMx

SFMx found (%)a

Nominal concentration (er) Paired
SFMx (mg mL–1) Reported method Proposed (%) t-test
(21) methodb
1.0 99.7 ± 1.8 97.3 ± 2.5 2.4 2.005
t = 2.41
F = 1.93
2.0 99.2 ± 0.9 99.6 ± 1.3 0.4
t = 0.75
F = 2.10
3.0 99.5 ± 1.2 99.7 ± 1.4 0.2
t = 0.35
F = 1.36
5.0 97.3 ± 1.2 97.9 ± 1.0 0.7
t = 1.70
F = 1.44
6.0 99.7 ± 1.0 100.8 ± 1.2 1.0
t = 2.12
F = 1.44
a Mean ± SD, n = 6.
b Tabular t-value for d.f. 5 is 2.571; Tabular F-value for d.f. 5 is 5.05.

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Pharm. 57 (2007) 333–342.

Table IV. Interference studies of commonly used excipients

Recovery (%)a,b
Conc.
Exicipient
(mg mL–1)
SFMx SFD SFA SFMt SFMr SFG
Gum acacia 5.0 99.5 ± 0.3 99.2 ± 0.3 100.5 ± 0.2 99.2 ± 0.3 100.1 ± 0.3 99.2 ± 0.3
Talc 5.0 100.1 ± 0.3 99.5 ± 0.3 99.2 ± 0.4 100.4 ± 0.3 100.1 ± 0.3 99.5 ± 0.3
Starch 5.0 99.2 ± 0.3 99.2 ± 0.3 99.2 ± 0.3 99.4 ± 0.2 100.2 ± 0.2 99.6 ± 0.3
Dextrose 3.5 99.2 ± 0.3 99.5 ± 0.3 99.6 ± 0.3 99.5 ± 0.3 99.6 ± 0.3 99.2 ± 0.3
Glucose 3.0 99.6 ± 0.3 99.5 ± 0.3 99.7 ± 0.2 99.2 ± 0.3 99.6 ± 0.3 95.5 ± 0.3
Lactose 4.0 100.2 ± 0.3 100.1 ± 0.3 100.2 ± 0.2 99.2 ± 0.5 100.7 ± 0.3 99.9 ± 0.2
Carboxymethyl- 4.0 100.5 ± 0.3 99.2 ± 0.2 100.2 ± 0.2 100.8 ± 0.4 100.6 ± 0.3 99.8 ± 0.4
cellulose
Magnesium 3.0 99.2 ± 0.3 99.2 ± 0.3 99.8 ± 0.2 99.7 ± 0.3 100.2 ± 0.2 99.9 ± 0.2
stearate
Sodium alginate 4.0 99.3 ± 0.6 99.6 ± 0.3 99.8 ± 0.3 99.2 ± 0.5 99.9 ± 0.2 99.1 ± 0.3
Vitamin B6 3.8 100.3 ± 0.3 100.2 ± 0.3 100.6 ± 0.3 100.7 ± 0.4 100.3 ± 0.3 100.2 ± 0.3
a Concentration of sulfonamide drug: 4 ìg mL–1.
b Mean ± SD, n = 6.

The reported methods and the proposed method are compared in Table VI. For ex-
ample, the proposed method is more simple and sensitive than the method including
drug diazotization coupling with dopamine followed by complexation with molybdate
ion reported earlier (28).

Table V. Determination of sulfonamide derivatives in pharmaceutical preparations

Amount of drug found (in mg)a

Label
Sample Proposed BP Reported
claim t-value F-value
method method (4) method (21)
Septran 400 398.00 ± 0.70 397.00 ± 0.60 397.00 ± 0.80 2.29 1.44
(mg SFMx)
Sulphadiazine 500 497.00 ± 0.50 496.00 ± 0.60 496.00 ± 0.80 2.29 1.44
(mg SFD)
Albucid 10 9.90 ± 0.30 9.90 ± 0.30 9.75 ± 0.30 2.48 2.25
(mg mL–1 SFA)
Locula 10 9.85 ± 0.20 9.80 ± 0.30 9.78 ± 0.30 2.50 1.96
(mg mL–1 SFA)
a Mean ± SD, n = 6.

Theoretical t-value = 2.776; theoretical F-value = 6.39.

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P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

Table VI. Comparison of reported spectrophotometric methods with the proposed method

Beer’s law Molar

Reagent(s) Sulfonamide ëmax
limits absorptivity Reference Remark
used analyzed (nm)
(mg mL–1) (L mol–1 cm–1)
p-Benzoquinone SFMx 500 10–50 25 heating is needed
and SFD
o-Chloranil SFA 525 10–70 26
Phenol SFG 450 Not 1.65 ´ 104 27
and sodium reported
hypochlorite
Dopamine SFMx 500 0.1–7.0 2.67 ´ 104 28 diazotisation cou-
pling, product is
complexaton with
molybdate
8-Hydroxy- SFMx 500 0.2–6.0 3.38 ´ 104 this diazotization of
quinoline paper drug followed by
(8-HQ) coupling with 8-HQ

The proposed method was found to be simple, rapid, selective and more sensitive
than most of the spectrophotometric methods available in literature. It does not involve
heating, extraction and consumes less time. The products are stable for a sufficient inter-
val of time making the method useful in practice.

CONCLUSIONS

The proposed method is simple, sensitive and free from drastic experimental condi-
tions such as heating. It is also accurate and precise enough to be successfully adopted
as an alternative to the existing spectrophotometric method and evaluation of drugs in
pharmaceutical preparations to assure a high standard of quality control.
Acknowledgements. – One of the authors (Shailendra D. Naik) thanks the University of Mysore
for the support to this research work.

REFERENCES

1. L. A. Mitscher, Antibiotics and Antimicrobial Agents, in Foye’s Principles of Medicinal Chemistry

(Eds. D. A. Williams and T. L. Lemke), 5th ed., Lippincott Williams and Wilkins, Philadelphia
2002, pp. 819–862.
2. W. A. Petri, Jr., Antimicrobial Agents, in Goodman and Gilman’s Pharmacological Basis of Therapeu-
tics (Eds. J. G. Hardman and Lee E. Limbird), 10th Ed., McGraw Hill, New York 2001, pp. 1171–
1188.

340
P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

3. J. M. Beale, Jr., Anti Infective Agents, in Wilson and Gisvold’s Text Book of Organic Medicinal and
Pharmaceutical Chemistry (Eds. J. H. Block and J. M. Beale, Jr.), 11th ed., Lippincott William and
Wilkins, Philadelphia 2004, pp. 217–281.
4. British Pharmacopoeia, Vol II, Her Majesty’s Stationery Office, London 2004, pp. 1858–1859.
5. B. Chivarino, M. A. Crestoni, A. Di-Marzio and S. Fornarini, Determination of sulfonamide an-
tibiotics by gas chromatography coupled with atomic emission detection, J. Chromatogr. Biomed.
Appl. 706 (1998) 269–277; DOI: 10.1016/S0378–4347(97)00568–9.
6. F. M. El Anwar, A. M. El Walily, M. H. Abdel Hay and M. El Swify, The analysis of a triple sul-
fonamide in pharmaceutical powder form by HPLC, Anal. Lett. 24 (1991) 767–779; DOI: 10.1080/
00032719108052941.
7. G. K. Thomas, R. G. Millar and P. W. Antis, Stability of sulfonamide antibiotics in spiked pig
liver tissue during frozen storage, JAOAC Int. 80 (1997) 988–995.
8. G. Knupp, H. Pollmann and D. Jonas, An improved HPTLC method for the rapid identification
and quantification of sulfonamides, Chromatographia 22 (1986) 21–24; DOI: 10.1007/BF02257291.
9. C. L. Flurer, Analysis of antibiotics by capillary electrophoresis, Electrophoresis 18 (1997) 2427–
2437; DOI: 10.1002/elps.1150181233.
10. F. Malecki and V. Starosak, Potentiometric determination of sulfonamides with a silver sulfide
electrode, Anal. Chim. Acta 139 (1982) 353–357; DOI:10.1016/S0003–2670(01)94015–2.
11. M. T. Ackermans, J. L. Beckers, F. M. Everaerts, H. Hoogland and M. J. H. Tomassen, Determi-
nation of sulphonamides in pork meat extracts by capillary zone electrophoresis, J. Chromatogr.
596 (1992) 101–109; DOI: 10.1016/0021–9673(92)80209–D.
12. T. A. M. Msagati and J. C. Ngila, Voltammetric detection of sulfonamides at a poly(3-methyl-
thiophene) electrode, Talanta 58 (2002) 605–610; DOI: 10.1016/S0039–9140(02)00327–2.
13. E. Martlbauer, E. Usleber, E. Schneider and R. Dietrich, Immunochemical detection of antibiot-
ics and sulfonamides, Analyst 119 (1994) 2543–2548; DOI: 10.1039/AN9941902543.
14. S. W. Garden and P. Sporns, Development and evaluation of an enzyme immunoassay for sul-
famerazine in milk, J. Agric. Food Chem. 42 (1994) 1379–1391; DOI: 10.1021/jf00042a026.
15. M. S. Pena, F. Salinas, M. C. Mahendero and J. J. Aaron, Spectrofluorimetric determination of
sulphonamides in pharmaceutical compounds and foods, J. Pharm. Biomed. Anal. 10 (1992) 805–
808; DOI:10.1016/0731–7085(91)80084–M.
16. Y. M. Issa, A. L. El. Ansary and W. Selim, Enthalpimetric determination of sulfa drugs in pure form
and pharmaceutical formulations, Anal. Lett. 31 (1998) 131–146; DOI: 10.1080/00032719808001838.
17. W. S. Sutherland, J. J. Laserna, M. J. Angebranndt and J. D. Winefordner, Surface-enhanced Ra-
man analysis of sulfa drugs on colloidal silver dispersion, Anal. Chem. 62 (1990) 689–693; DOI:
10.1021/ac00206a008.
18. P. Nagaraja, K. R. Sunitha, R. A. Vasantha and H. S. Yathirajan, Iminodibenzyl as a novel cou-
pling agent for the spectrophotometric determination of sulfonamide derivatives, Eur. J. Pharm.
Biopharm. 53 (2002) 187–192; DOI:10.1016/S0939–6411(01)00235–1.
19. P. Nagaraja, H. S. Yathirajan, C. R. Raju, R. A. Vasantha, M. S. Hemantha Kumar and P. Nagend-
ra, 3-Aminophenol as a novel coupling agent for the spectrophotometric determination of sul-
fonamide derivatives, Farmaco 58 (2003) 1295–1300; DOI: 10.1016/S0014–827X (03) 00093–4.
20. S. Raghuveer, I. R. K. Raju, D. K. Vastu and C. M. R. Shrivastava, Colorimetric determination of
sulphamethoxazole in pharmaceutical preparations, Indian Drugs 30 (1993) 132–135.
21. A. S. Amin and M. M. Zarch, Acetylacetone-formaldehyde reagent for the spectrophotometric
determination of some sulfa drugs in pure and dosage forms, Mikrochim. Acta. 124 (1996) 227–
233; DOI: 10.1007/BF01242820.

341
P. Nagaraja et al.: A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations, Acta
Pharm. 57 (2007) 333–342.

22. S. S. Sabry, Enhanced spectrophotometry of sulfonamides with 2-acetylbutyrolactone derivatives,

Anal. Lett. 39 (2006) 2591–2615; DOI: 10.1080/00032710600824748.
23. ICH Topic Q2(R1), Validation of Analytical Procedures: Text and Methodology (CPMP/ICH/281/95)
acessed October 27, 2006.
24. R. A. Day, Jr. and A. L. Underwood, Errors and the Treatment of Analytical Data, in Quantitative
Analysis, 6th ed., Prentice-Hall of India, New Delhi 1999, pp. 7–42.
25. A. M. Mohamed, H. F. Askal and G. M. Saleh, Use of p-benzoquinone for the spectrophotometric
determination of certain sulphonamides, J. Pharm. Biomed. Anal. 9 (1991) 531–538; DOI: 10.1016/
0731–7085(91) 80174–8.
26. G. R. Rao, S. S. N. Murthy, P. J. Rao and I. R. K. Raju, Spectrophotometric determination of sul-
phacetamide sodium with o-chloranil in dosage form, Indian J. Pharm. Sci. 50 (1988) 138–140.
27. A. G. Fogg and N. M. Fayad, Spectrophotometric and differential pulse polarographic determi-
nation of sulphaguanidine by reaction with hypochlorite and phenol, Anal. Chim. Acta. 106
(1979) 365–367; DOI:10.1016/S0003–2670(01)85022–4.
28. P. Nagaraja, H. S. Yathirajan, K. R. Sunitha and R. A. Vasantha, A new sensitive and rapid spec-
trophotometric method for the determination of sulfa drugs, JAOAC Int. 85 (2002) 869–874.

S A @ E TA K

Osjetljiva spektrofotometrijska metoda za odre|ivanje sulfonamida

u farmaceutskim pripravcima
PADMARAJAIAH NAGARAJA, SHAILENDRA D. NAIK, ASHWINEE KUMAR SHRESTHA
i ANANTHARAMAN SHIVAKUMAR

U radu je opisana nova, jednostavna i osjetljiva spektrofotometrijska metoda za od-

re|ivanje sulfonamida. Metoda se temelji na prevo|enju sulfacetamida, sulfadiazina, sul-
fagvanidina, sulfamerazina, sulfometazina i sulfametoksazola u diazoderivate koji kon-
denzacijom s 8-hidroksikinolinom u alkalnom mediju daju crveno obojene produkte s
maksimumom apsorpcije pri 500 nm. Beerov zakon vrijedi u koncentracijskom rasponu
0,1–7,0 mg mL–1. Granice kvantifikacije i granice detekcije su 0,11–0,18, odnosno 0,03–0,5
mg mL–1. Za predlo`enu metodu procijenjena je intermedijarska preciznost (RSD 0,1–0,5%) i
to~nost (analiti~ki povrat 97,3–100,8). Uobi~anjene pomo}ne tvari u tabletama ne inter-
feriraju tijekom odre|ivanja. Metoda je uspje{no primijenjena za analizu sulfonamida u
farmaceutskim pripravcima.

Klju~ne rije~i: sulfonamidi, diazotacija, 8-hidroksikinolin, spektrofotometrija, farmaceutski pripravak

Department of Studies in Chemistry, University of Mysore, Manasagangothri, Mysore-570006, India

Charak Pharma Pvt. Ltd., Silvassa, U. T. of Dadra Nagar Haveli, Silvassa-396230, India

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