Derivative Spectrophotometric method for Estimation of Secnidazole in Bulk and Pharmaceutical Dosage form
Rajan V. Rele*
Central Research Laboratory, D. G. Ruparel College, Matunga, Mumbai 400016
*CorrespondingAuthorE-mail: drvinraj@gmail.com
ABSTRACT:
It is used mainly to treat intestinal ameobiasis, fiardiasis, trichomoniasis and bacterial vaginosis. All such disease symptoms are treated with a single once only dose of such drug.
According to the literature review several methods has been developed for drug, like spectroscopy methods1-3. HPLC4-9, HPTLC10. The proposed aim of the study was to develop simple, accurate, specific and precise UV spectrophotometric method for the estimation of drug in the bulk and pharmaceutical formulation
MATERIALS AND METHOD:
Instrument and reagents:
Spectral scan was made on a Shimadzu UV-spectrophotometer, model 1800 (Shimadzu, Japan) with spectral band width of 0.5 nm with automatic wavelength corrections by using a pair of 10 mm quartz cells. All spectral measurements were done by using UV-Probe 2.42 software.
Reference standard of secinadazole was obtained from reputed firm with certificate of analysis. Hydrochloric acid was used of AR grade.
Preparation of standard drug solutions:
About 10 mg of standard secnidazole was weighed accurately and transferred in 100 ml of volumetric flask. About 30 ml of distilled water was added and sonicated for 15 minutes. The volume was adjusted up to the mark with distilled water to give concentration as 100 μg /ml.
Estimation from tablets:
Twenty tablets were weighed accurately and average weight of each tablet was determined. Powder equivalent to 10 mg of secnidazole was weighed and transferred in 100 ml of volumetric flask. A 30 ml of distilled water was added and sonicated for 15 minutes and filtered. The filtrate and washing were diluted up to the mark with distilled water to give concentration as 100 μg /ml. Such solution was used for analysis.
EXPERIMENTAL:
Method: First order derivative method:
For the selection of analytical wavelength, 10 μg/ml solution of secinadazole was scanned in the spectrum mode from 370 nm to 200 nm by using distilled water as blank. The first order derivative spectrum was obtained by using derivative mode by UV probe 2.42 software. From the spectrum, the amplitude of the derivative spectrum was measured at 305 nm.
Preparation of calibration curves:
Series of solutions containing 2.5–15 µg/ ml of secnidazole were used to determine linearity of the proposed method respectively. Solutions were scanned in the spectrum mode and absorbance spectra were converted to first order derivative spectra [Fig. 1(a), 1(b)].
Range of 10 µg/ ml.
Fig. 1: spectrum of first order derivative of secnidazole in the concentration.
After observing the overlain first order derivative spectra of secnidazole, wave length selected was 305 nm, where secnidazole showed considerable absorbance. The calibration curves were plotted of dA/ dλ against concentrations [Fig. 2 ].
Fig.2 : Calibration curve of secnidazole in the concentration range of 2.5-15 µg/ml.
Results of the analysis are given in table 1.
Table 1: Values of results of optical and regression of drugs
|
Parameter |
First order derivative |
|
Detection Wavelength (nm) |
305 |
|
Beer Law Limits (µg/ml) |
2.5-15 |
|
Correlation coefficient(r2) |
0.9999 |
|
Regression equation (y=b+ac) |
|
|
Slope (a) |
0.001 |
|
Intercept (b) |
0.001 |
Estimation from tablets:
Twenty tablets were weighed accurately and average weight of each tablet was determined. Powder equivalent to 10 mg of secnidazole was weighed and transferred in 100 ml of volumetric flask. A 30 ml of distilled water was added and sonicated for 15 minutes and filtered. The filtrate and washing were diluted up to the mark with distilled water to give concentration as 100 μg /ml of each drug. Such solution was scanned in the range of 200-370 nm against distilled water as blank. The absorbance spectra were converted to first order derivative spectra. Calculations were done as per the equations. The concentrations of secnidazole present in tablets were calculated by substituting the values of absorbance in linearity equations.
For first order derivative method, Y = 0.001x + 0.001
Method Validation:
These methods were validated according to ICH guidelines.
Accuracy:
To ascertain the accuracy of proposed methods, recovery studies were carried out by standard addition method at three different levels (75%, 100% and 125%). Percent recovery for secnidazole was found in the range of 99.61 % to 100.47 for first order derivative method respectively. (Table 2).
Table 2: Statistical evaluation of the data subjected to accuracy for first order derivative method.
|
Level of % recovery |
Amount present in µg/ml |
Amount added in µg/ml |
Amount found in µg/ml |
% Recovery |
Mean % recovery |
|
75% |
2.5 |
5.0 |
7.501 |
100.013 |
99.97
|
|
2.5 |
5.0 |
7.428 |
99.04 |
||
|
2.5 |
5.0 |
7.571 |
100.94 |
||
|
100% |
2.5 |
7.5 |
10.071 |
100.71 |
100.47
|
|
2.5 |
7.5 |
10.142 |
101.42 |
||
|
2.5 |
7.5 |
9.928 |
99.28 |
||
|
125% |
2.5 |
10 |
12.428 |
99.424 |
99.616
|
|
2.5 |
10 |
12.571 |
100.568 |
||
|
2.5 |
10 |
12.357 |
98.856 |
||
|
% R.S.D. |
0.922543 |
100.01
|
|||
Linearity:
The linearity of measurement was evaluated by analyzing different concentration of the standard solutions of secnidazole in the range of 2.5-15 µg/ml for first order derivative respectively.
Precision:
The method precision was established by carrying out the analysis of tablets powder blend containing 500 mg of secnidazole. The assay was carried out for the drugs by using proposed analytical method in six replicates. The values of relative standard deviation were well within limits 0.8502 % respectively indicating the sample repeatability of the methods. The results obtained are tabulated in table 3.
Table 3: Statistical evaluation of the data subjected to method of precision
|
Sr. No. |
Sample No. |
Percentage recovery (%) |
|
1 |
1 |
100.71 |
|
2 |
2 |
100.70 |
|
3 |
3 |
99.88 |
|
4 |
4 |
99.28 |
|
5 |
5 |
101.44 |
|
6 |
6 |
101.42 |
|
Mean % assay |
0.8551 |
|
|
%R.S.D. |
0.8502 |
|
Intra-day precision was estimated by assaying tablets powder blend containing 500 mg of secnidazole. The assay was carried out for the drugs by using proposed analytical method in six replicates. The results were average for statistical evaluation.
Inter-day precision was estimated by assaying tablets powder blend containing 200 mg of secnidazole for three consecutive days (i.e. 1st, 3rd and 5th days). The statistical validation data for intra and inter day precision is summarized in table 4.
Table 4: Summary of validation parameter for intra-day and inter-day
|
Sr. No. |
Parameters |
First order derivative |
|
1 |
Intra-day precision (N=3)amount found ± % R.S.D. |
99.23%
0.2562 |
|
2 |
Inter-day precision (N=3)amount found ± % R.S.D. |
99.128
0.2431 |
Both intra- day and inter-day precision variation found to be less in % RSD values. It indicates high degree of precision of the method.
RESULT AND DISCUSSION:
The developed first derivative spectrophotometric methods for determination of secnidazole in tablet formulation was found to be simple and convenient for the routine analysis of drug. The proposed method is accurate, precise and reproducible. It is confirmed from validation data as given in tables 1 to 4. The % RSD was found to be less than 1, which indicates validity of method. Linearity was observed by linear regression equation method for secnidazole in different concentration range. The correlation coefficient of these drugs was found to be close to 1.00, indicating good linearity figure 2.
The assay results obtained by proposed method is shown in table 2 are in good agreement. Hence proposed method can be used for routine analysis pharmaceutical dosage form. Methods are simple, accurate, precise, reliable, rapid, sensitive, reproducible and economical. It is validate as per ICH guidelines.
The proposed method is simple, precise, accurate and rapid for the determination of secnidazole pharmaceutical dosage form. The methods do not require any ratio of first derivative. The amplitude of first derivative can be directly used to assay of formulation. This method can be adopted as an alternative to the existing methods. It can be easily and conveniently adopted for routine quality control analysis.
ACKNOWLEDGEMENT:
Authors express sincere thanks to the Principal of D.G. Ruparel College, Dr. Tushar Desai, for encouragement and providing laboratory facilities.
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Received on 05.02.2019 Modified on 18.02.2019
Accepted on 05.03.2019 ©AJRC All right reserved
Asian J. Research Chem. 2019; 12(2):71-74.
DOI: 10.5958/0974-4150.2019.00016.6