Hindustan Abdul Ahad et al.

/ Journal of Pharmacy Research 2011,4(3),739-740

Research Article
ISSN: 0974-6943 Available online through
www.jpronline.info
Spectrophotometric Determination of Cefadroxil in Pharmaceuticals Dosage Forms by
Bromination Method
Mallapu Rani E1*, Hindustan Abdul Ahad2*, Sreenivasulu R 2, Mahendra Kumar P2, Akula Ashwan Kumar 3, Siddaiah G 2
1
Department of Chemistry, Rayalaseema University, Kurnool, Andhra Pradesh, India
2
Department of Pharmacy, College of pharmacy, Sri Krishnadevaraya University, Anantapur- 515003, Andhra Pradesh, INDIA,
3
Department of Pharmacy, Bharat Institute of Technology, Hyderabad
Received on: 27-10-2010; Revised on: 15-12-2010; Accepted on:24-02-2011
ABSTRACT
A Spectrophotometric method is described for assay of Cefadroxil in tablets. In this method, the Cefadroxil was brominated with bromate – bromide mixture under strong acidic conditions.
After bromination, the excess brominating mixture was treated with methylene blue result in formation of stable grass green coloured complex. The absorbance of the grass green colour was
measured at 670 nm against the blank solution. Results of analysis were validated statistically and by recovery studies. The proposed method is successfully applied to the determination of
Cefadroxil in tablets.

Key words:Cefadroxil, bromate, absorbance, Spectrophotometric method, methylene blue.

INTRODUCTION
Cefadroxil is chemically, (6R, 7R), -7-[(2R) -2- amino-
2- (4 - hydroxyl phenyl) acetyl) amuni] -3- methyl -
8-0X0-5-thia -1-azbicyclo [4.2.0]oet-2 ene -2-carboxy-
lic acid hydrate. It is freely soluble in chloroform and
methanol. It is commercially known as Droxil, Blue
drox and Cefadrox (Indian brands). It is used as an
antibiotic in treatment of various diseases. The struc-
ture of cefadroxil was shown in Fig.1.Survey of lit-
erature reveals that various methods were reported
for the estimation of cefadroxil in its pharmaceutical Fig. 1: Molecular structure of
formulations. Assay of cefadroxil have been devel- Cefadroxil drug
oped by sensitive visible spectrophotometric method1. Cefadroxil and Cefuroxime in human
urine were determined (using first derivative) spectrophotometry and high performance liquid
chlomatography2-3.
A wide range of chromato graphic techniques such as isocratic High Performance Liquid
Chromatography, Reversed phase column liquid chromatography, sensitive kinetic spectro-
photometry, sequential injection analysis and spectrophotometric methods etc. 4-8
The present investigation was under taken with the developing simple, rapid and accurate
method. This method is based on the oxidation-bromination reaction of the drug by bromine
generated by the action of acid on a bromate bromide mixture 9, 10.
MATERIALS AND METHODS
Materials
Apparatus
Spectronics 1001 Spectrophotometer with 10 mm Matched quartz cuvettes used for absorbance
values of the drug solution.
Reagents
All employed chemicals were of analytical grade, and all solutions were freshly prepared in
double distilled water.
Bromate – bromide mixture (0.1NKBro3-0.1NKBr)
0.278 g of KBro3 and 1.5g of KBr were dissolved in 10 ml of distilled water and the volume
was made up to 100 ml with distilled water.
Hydrochloric acid solution (4N)
Hydrochloric acid solution (4N) is prepared by diluting the requisite volume of concentrated
AR hydrochloric acid (Ranbaxy, Mumbai, India) i.e. 36.36 ml of concentrated AR hydrochlo-
ric acid diluting 100 ml of double distilled water.
Methylene Blue solution (1%)
1g of AR methylene Blue (Ranbaxy, Mumbai, India) was dissolved in double distilled water
and the resulting solution is made up to the mark in the 100 ml standard flask with distilled
water.
Preparation of Cefadroxil standard solution
50 mg of Cefadroxil was dissolved in methanol and the volume was adjusted to 50ml with
methanol in 50 ml standard flask. Then 10 ml drug solution was made up to the mark in the
50 ml standard flask with methanol, to give a working concentration of 200 µg / ml.
Spectrophotometric determination of Cefadroxil
This method was applied to the estimations of the drug dosage forms were purchased from local
commercial sources and subjected to analysis. The contents of tablets were accurately weighed
and ground into a fine powder. A quantity of the powder equivalent to 50mg was taken in 50
ml volumetric flask, dissolved in methanol and volume was made up to 50 ml with methanol
to get concentration of 1 mg/ml. The stock solution was further diluted to obtain working
concentration of 200 µg / ml.
Different aliquots of 1 ml, 2 ml, 3 ml and 4 ml of the working drug solution are transferred into
a series of 25 ml volumetric standard flasks. To each flask 2 ml of 4N Hydrochloric acid and 2
ml of 0.02N brominating mixture (or) bromate – bromide mixture are added. The contents in
each flask are thoroughly mixed and allowed to stand for five minutes at room temperature for
complete bromination orange coloured solution was formed. Then 1 ml of 1% methylene blue
solution was added each flasks and the resultant solution was diluted with methanol and mixed
thoroughly to get a solution of uniform light grass green colour. After 5 minutes the absorbance
was measured at 670 nm against blank solution. A calibration curve was plotted between the
absorbance values and amount of the drug.
Method Validation
This method was validated in terms of linearity, accuracy and precision and reproducibility of
the sample applications. A linear relation was found between absorbance and concentration in
the ranges. Beer’s law was obeyed in the concentration ranges.
Statistical analysis
A Statistical analysis was performed on the statistically significant variables using the statisti-
cal software. The Co-efficient of variation, standard deviation and student t-test were deter-
mined.
The Standard deviation and t-test of the Cefadroxil was calculated from five measurements of
replicate samples. The values of Statistical analysis were shown in Table 1. The values of
standard deviation and coefficient variation are low, indicates high accuracy and reproducibility
of the method. The calculated ‘t’ values are less than ‘t’ theoretical values with 4(x-1=5-1)
degrees of freedom at 5-1. Level of significance indicates that there is no significant difference
between proposed method and standard method.
Table 1: Drug concentration and Absorbance values for Cefadroxil standard curve
Drug concentration(µg) Absorbance

100 0.067±0.003
*Corresponding author. 200 0.095±0.002
400 0.167±0.004
Hindustan Abdul Ahad 2 600 0.197±0.015
Department of Pharmacy, College of pharmacy, Sri 800 0.268±0.003
Krishnadevaraya University, Anantapur- 515003, Andhra
Pradesh, INDIA RESULTS AND DISCUSSION
Tel.: +91 8554 255890 The standard calibration values and curve were tabulated in Table 2 and shown in Fig.2. The
Fax.: +918554255244
E-mail:abdulhindustan@rediffmail.com
Journal of Pharmacy Research Vol.4.Issue 3. March 2011 739-740
 Hindustan Abdul Ahad et al. / Journal of Pharmacy Research 2011,4(3),739-740
Table 2: Assay of Cefadroxil in tablets In the present proposed method, Cefadroxil is treated with known potassium bromate-
potassium bromide excess of brominating mixture in acidic medium. The drug undergoes
Sample Labeled amount Amount found Recovery
(mg/tab) (mg/tab) (%) bromination it forms uniform orange coloured solution. These contents are thoroughly mixed
and allowed to stand for five minutes at room temperature for complete bromination. Then
Tablet – 1 250 249.96 99.6 treated with 1% of methylene blue at 670 nm the standard deviation and coefficient of variation
Tablet – 2 250 250.06 100.02
Tablet – 3 250 248.84 99.93 are low, indicates high accuracy and reproducibility of this method. The data assay values of
commercial formulations were subjected to statistical evaluation for student‘t’ test to study the
proposed method. The calculated ‘t’ values are less than ‘t’ theoretical values. Hence the
proposed assay of drug content of the sample was estimated of drug content of the sample was
estimated from the calibration curve. The assay values of Cefadroxil were shown in Table-2.
The Statistical analytical data of Cefadroxil was shown in Table 1.

CONCLUSION
The proposed spectrophotometric method was found to be simple, precise, accurate and less
time consuming. Hence the assay results to demonstrate that it is possible to use a bromate-
bromide solution as an oxidimetric and brominating agent for the determination of Cefadroxil
in pharmaceutical formulations.

REFERENCES
1. Chilkuri S.P. Sastry, Assay of cisapride in pharmaceutical formulations by visible spectrophotometry,
Fig: 2: Standard calibration curve for Cefadroxil Publisher Springer Wien, Volume 126, Numbers 1-2 / March, 1997, 63 – 67.
2. El-Gindy A, First-derivative spectrophotometric and LC determination of cefuroxime and cefadroxil in
urine, Journal of pharmaceutical and biomedical analysis, 2000, vol. 23, 2-3, pp. 341-352.
Table 3: Statistical analysis of the determination of Cefadroxil 3. Haresh M. Patel, Determination of Cefadroxil in Bulk Powder and its Dosage Forms by Spectrophoto-
Sample S.D* C.V* * t a
T b metric Method, Clinical Chemistry, American Association for Clinical Chemistry, Vol 33, 1987, 1788-
cal tab 1790.
4. Helaleh M.I.H., Abu-Nameh E.S.M., A kinetic approach for determination of cefadroxil in pharmaceu-
ticals by alkaline hydrolysis, Journal of AOAC International, 1998, vol. 81, 3, pp. 528-533 .
Tablet – 1 0.4159 0.1663 0.2147 2.78 5. Hendrix C, Comparative study of liquid chromatographic methods for the determination of cefadroxil,
Tablet – 2 0.8502 0.3399 0.1578
Journal of chromatography, 1993, vol. 634, 2, pp. 257-261.
Tablet – 3 0.7300 0.2921 0.4901
6. Hsu MC, Column liquid chromatography and microbiological assay compared for determination of
cefadroxil preparations, 1992 Sep 18; 609(1-2):181-6.
* Standard deviation; * * coefficient of variation; ‘a’ Calculated ‘t’ value by proposed Method; 7. JA Mc Ateer et al., Liquid-chromatographic determination of five orally active cephalosporins-cefixime,
cefaclor, cefadroxil, cephalexin and cephradine-in human serum, Clinical Chemistry, American Asso-
‘b’ Theoretical values at 95% confidence limit ciation for Clinical Chemistry. Vol 33, 1987, 1720-1740.
8. Welling P G et al., A pharmacokinetic comparison of cephalexin and cefadroxil using HPLC assay
present study was carried out to develop a simple, rapid, sensitive, precise, reproducible and procedures, 1985 Apr-Jun;6(2):147-57.
9. Jirayu Makchit et al., Determination of Cefadroxil by Sequential Injection with Spectrophotometric
accurate spectrophotometric method for the estimation of Cefadroxil in pharmaceutical dosage Detector, Anal. Sci., Vol. 22, p.591, (2006) .
forms. 10. Ronald J. Gorski et al., Determination of Cefsulodin, Cefmenoxime, and Cefadroxil as Residues on
Surfaces, Publisher Springer Netherlands, Volume 8, Number 12 / December, 1991, Pages 1525-1527.

Source of support: Nil, Conflict of interest: None Declared

Journal of Pharmacy Research Vol.4.Issue 3. March 2011 739-740