Ibuprofeno 4
Ibuprofeno 4
Ibuprofeno 4
a www.pelagiaresearchlibrary.com
ISSN: 0976-8688
CODEN (USA): PSHIBD
ABSTRACT
A new simple, accurate, precise and reproducible a reverse phase high performance (RP RP-HPLC) method has been
developed of ibuprofen in tablet dosage forms using C18 column (Hypersil BDS, 150 x 4.6 mm, 5 m) in isocratic
mode. The mobile phase contains a combination of Acetate buffer (triethylamine & ortho phosphoric acid ) and
acetonitrile in the ratio of 40:60%
% (v/v). The flow rate was 1.5 ml/min and detection wavelength
avelength was carried out at
220 nm. The retention times of ibuprofen was 3.2 min,, respectively. The validation of method was carried out
utilizing ICH guidelines. The described HPLC method was successfully employed for the analysis of pharmaceutical
formulations containing Tablet dosage form.
INTRODUCTION
The main aim of the present work is to develop stability indicating RP-HPLC
HPLC method for the quantitative estimation
of Ibuprofen in pharmaceutical formulations such as tablet dosage forms etc. S (+) Ibuprofen form is not official in
any pharmacopoeias but literature survey reveals that there are limited techniques for the estimation of ibuprofen in
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tablet form using HPLC method [5-13]. Current research work mainly devoted to develop a simple, rapid, precise,
accurate and reproducible isocratic RP-HPLC method for the determination of ibuprofen and the developed method
is partialy validated with respect to specificity, linearity, precision, accuracy [14] .
EXPERIMENTAL
I. Chemicals and Reagents:
Sample of ibuprofen pure drug was received from M/S Medreich Private Limited, Bangalore, India and tablet
dosage form was purchased from market manufactured by M/S Genovo Development Services Ltd, Bangalore,
India. HPLC grade acetonitrile, ortho-phosphoric acid were purchased from M/S Rankem , Mumbai,
India.Triethylamine was purchased from M/S Rankem Mumbai, India.High pure water was prepared by using
Millipore, Milli Q plus (TKA) purification system.
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Method precision [21]:
The method precision was performed by preparing six replicate sample preparations as per testing procedure and
injected in to the chromatography.The percentage w/w of ibuprofen was calculated from six replicates and %RSD.
Specificity [22,23]:
The specificity of the method was determined by analysing the interference of placebo was conducted. It was
performed on Ibuprofen placebo in duplicate, equivalent to the weight of placebo present in portion of test
preparation as per the test method and the impurity interference of Ibuprofen impurities by preparing individual
impurity solution and mixed impurity solution at Specification level (0.2% for Ibuprofen impurities). Impurity
spiked test solution of Ibuprofen tablet at 1% level of all impurities was injected into the HPLC. No interference was
detected at the retention time of Ibuprofen in sample solution.
Linearity [23,24]:
Linearity was studied to determined by plotting a graph between concentration on X-axis and peak area on Y-axis,
the correlation coefficient was determined. Five different concentrations of Ibuprofen working standard ranging
from 4.06 g/ml to 12.181 g/ml were prepared and analyzed as per test method. Calibration curve was constructed
by plotting average peak area versus concentrations and regression equation was computed for the drug.
The current RP-HPLC technique is most accurate, reliable and precise method of analysis for the quantitative
estimation of ibuprofen from its pharmaceutical formulations and dosage form. The specificity of the method was
initially performed by injecting impurities and placebo in to the chromatography to check the contribution at the
detection wavelength. The current method system suitability was accounted by measuring USP tailing factor, USP
Plate count for the peak of Ibuprofen from Standard Solution and percentage RSD of Area for the peak of Ibuprofen
from six replicate injection of Standard Solution. The obtained values are 1.0 as USP tailing factor (should be not
more than 2.0), 8190 as USP Plate count (should be not less than 2000) and percentage RSD of area as 0.1(should be
not more than 2.0). The typical ibuprofen retention time in the current developed method was about 5 minutes. All
variations resulted with the very good percentage RSD of Assay i.e. less than 1.0%.
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Figure 3: RP-HPLC chromatogram of standard solution at 220 nm
Acceptance
System Suitability Parameters Observed value
Criteria
Theoretical plate count for Ibuprofen peak from first injection of standard solution. 8190 NLT 2000
The tailing factor for Ibuprofen peak from first injection of standard solution. 1.0 NMT 2.0
The Relative standard deviation for Ibuprofen peak response from five replicate injections of standard solution. 0.1 NMT 2.0
Table 3: % Assay and %RSD values of Ibuprofen for Method Precision test
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Sovan Pattanaik et al Der Pharmacia Sinica, 2013, 4(4):91-96
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Table 4: Placebo Interference in specificity of Ibuprofen
Potency (%)
Stock weight taken (mg) 40.70 Volume Taken (ml) 10 99.76
(as such basis)
Volume (ml) 100 Dil. To (ml) 50 Stock (g/ml) 81.2046
mg
Sample No. Level mg added % Recovery Mean % Recovery %RSD
Found
1 50% 100 101.989 101.60
2 50% 100 101.88 100.26 101.1 0.7
3 50% 100 101.933 101.33
4 100% 100 101.230 101.231
5 100% 100 101.570 101.575 101.5 0.2
6 100% 100 101.710 101.708
7 150% 100 101.79 101.04
8 150% 100 101.88 101.97 101.7 0.5
9 150% 100 101.95 101.96
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CONCLUSION
The main focus of this research article was developed and validated for the quantification of ibuprofen in bulk drug
and pharmaceutical formulations such as tablet. The method gave good resolution for the drug with a short analysis
time 5 minutes. The developed method was validated by using various validation parameters like accuracy, precision,
linearity, specificity. All the validation parameters were found to be well within the acceptance criteria. It is shown
that the method was accurate, reproducible, repeatable, linear, precise, and selective, proving the reliability of the
method [26,27,28]. These results show the method could find practical application as a quality control tool for
analysis of the drug in its Tablet dosage forms in quality control laboratories.
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