Methods Development and Validation of Cefprozil by UV-Vis Spectrophotometry
Thorat D.B*
PERS, Institute of Pharmacy, Loni (kd), Tal-Rahata, Dist- A’nagar (MS).
*Corresponding Author E-mail: dattatraya_thorat@rediffmail.com
ABSTRACT:
The present work describes which deals to developed and validate a simple, accurate, precise, economically effective US-VIS Spectrophotometric method for the estimation of cefprozil. These methods are developing using 280nm as the λmax of cefprozil respectively. Calibration curves were linear over the concentration ranges of 10-50µg/ml. These result demonstrate that the procedure is accurate, precise and reproducible (relatively standard deviation ≥1%) while being simple cheap and less time consuming and hence can be suitably applied for validation of these drug in laboratory.
KEYWORDS: Cefprozil, λmax, UV-VIS Spectroscopy.
INTRODUCTION:
Cefprozil is chemically (6R, 7R)-7-((R)-2-amino-2-(p-hydroxyl-phenyl) acetamido)-8-oxo -3-propenyl-5-thia-1-azabicyclo (4.2.0) oct-2-ene-2-carboxylic acid. Cefprozil is a semi synthetic broad-spectrum cephalosporin antibiotic, which is currently available in a oral dosage form (i.e. tablet and suspension) for the treatment of respiratory tract and skin or skin structure infection in both adults and children’s. The bactericidal action of cefprozil results from inhibition of cell wall synthesis. Literature survey reveals that HPLC method for the simultaneous determination of cefprozil diasteriomers, HPTLC for estimation cefprozil, Flow injection chemiluminscent determination of cefprozil spectrophotometric determination and spectroflurometric determinations of cefprozil have been developed.
EXPERIMENTAL PROCEDURE:
Materials:
UV-visible double beam spectrophotometer, spectroscan UV model 2600 version 6.67 having two match pair of quartz cells with 1cm path length.
Selection of common solvent:
After assessing the solubility of drugs in different solvents ethanol-water 50:50 has been selected as common solvent for developing methods.
Preparation of stock and calibration curve:
Standard stock solution of cefprozil was prepared by 0.174gm dissolve in 100ml of ethanol - water (50:50) gives 100ppm concentration.
From the above stock solution to make working standard solution of 10µg/ml UV-visible spectrophotometer in the range of 600-400nm.
Table 1: Result of accuracy studies
|
No. of preparation |
Concentration (ppm) formulation |
Pure drug |
% Recovery |
Mean |
SD |
% RSD |
|
80 % |
10 |
8 |
8.68 |
|
|
|
|
80% |
10 |
8 |
8.68 |
8.68 |
0.70 |
0.081 |
|
80% |
10 |
8 |
8.69 |
|
|
|
|
100 % |
10 |
10 |
8.082 |
|
|
|
|
100 % |
10 |
10 |
8.082 |
8.08 |
1.90 |
0.035 |
|
100% |
10 |
10 |
8.076 |
|
|
|
|
120% |
10 |
12 |
7.64 |
|
|
|
|
120% |
10 |
12 |
9.56 |
8.27 |
0.17 |
0.058 |
|
120% |
10 |
12 |
7.63 |
|
|
|
Validation:
Linearity:
Various aliquots were prepared from secondary stock solution (100ppm) ranging from 10-50ppm. The samples were scanned in UV – visible spectrophotometer against water-ethanol as blank. It was found that the selected drug shows linearity between the ranges of 10-50ppm.
Accuracy:
Solutions were prepared in triplicate at levels 80%, 100% and 120% of test concentration using cefprozil working standard as per the test method and taken absorbance of each solution in triplicate. The recovery result show that the proposed method has an acceptable level of accuracy of cefprozil which is from 80-120% of test concentration is 99.51-100.01%. Table 1.
Precision:
Precision was determined by studying the repeatability and intermediate precision. Precision of the method was demonstrated by intra-day and inter-day variation studies. In intraday study concentration of drugs were calculated on the same day at an interval of 3 hour. In inter day study the drug contents were calculated on three different days. In both intra and inter –day precision study for result mean, standard deviation and % RSD was calculated. It is given in table 3.
Ruggedness:
Ruggedness of the method was determined by carrying out the analysis by different analyst and the respective absorbance of 20ppm was noted. The result was indicated as %RSD and given in table 4.
RESULT AND DISCUSSION:
The developed method was found to be precise as % RSD values for intraday and inter-day were found to be less than 2%. Good recoveries of the drug were obtained at each added concentration, indicating that method was accurate. The method was also found to be specific indicated by % recoveries ranging from 7.64-9.56%. The method was also found to be rugged as indicated by the % RSD values which are less than 2%.
Table 2: Optical characteristics of data and validation parameter
|
Parameter |
Result |
|
Linearity |
1.40 |
|
Accuracy indicated by % recovery |
0.058 |
|
Precision indicated by % RSD |
1.04% |
|
Ruggedness indicated by % RSD |
0.17% |
|
Range |
10-50 ppm |
Table 3: Precision
|
Concentration (ppm) |
Absorbance |
SD |
% RSD |
|
10 |
0.847 |
0.468414 |
0.3492 |
|
20 |
0.775 |
0.47988 |
0.22169 |
|
30 |
1.864 |
3.44401 |
1.45268 |
Table 4: Ruggedness
Instrument 1 (Spectroscan uv model 2600)
|
Concentration (ppm) |
Absorbance |
Statistical analysis |
|
10 |
2.184 |
Mean – 0.41 |
|
20 |
2.141 |
S.D. – 0.20 |
|
30 |
2.184 |
%RSD – 0.13 |
|
40 |
2.156 |
|
|
50 |
2.615 |
|
Instrument 2 (SEMATZU)
|
Concentration(ppm) |
Absorbance |
Statistical analysis |
|
10 |
2.578 |
Mean – 1.13 |
|
20 |
4.000 |
S.D. – 0.56 |
|
30 |
4.000 |
%RSD – 0.22 |
|
40 |
4.000 |
|
|
50 |
4.000 |
|
CONCLUSION:
The methods reported here are found to be simple, sensitive, accurate and precise. Further spectrophotometric methods involve simple instrumentation which is cost effective compared with other instrumental techniques, which ordinary laboratories cannot afford to have. The present method involves the formation of highly stable colored species which may it easier for the determination of cefprozil from pharmaceutical dosage form in a routine manner.
ACKNOWLEDGEMENTS:
On the occasion of presenting this work, it my privilege to express my sincere thanks to PRES, Institute of Pharmacy, Loni Kd, and Pravara Rural College of Pharmacy, (Dept of Pharmaceutical Chemistry), Pravaranagar, Tal - Rahata, Dist - Ahmednagar (MS).
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Received on 15.10.2020 Revised on 21.01.2021
Accepted on 08.03.2021 ©Asian Pharma Press All Right Reserved
Asian Journal of Pharmaceutical Analysis. 2021; 11(2):70-72.
DOI: 10.52711/2231-5675.2021.00013