Vinay Wamorkar et al.

/ Journal of Pharmacy Research 2011,4(8),2633-2635

Research Article Available online through
ISSN: 0974-6943 http://jprsolutions.info
Validated Spectroscopic Method for Estimation of Naproxen from Tablet Formulation
Vinay Wamorkar*, Pendota Santhosh, Manjunth S. Y.
Department of Pharmaceutics, Srikrupa Institute of Pharmaceutical Sciences, Velkatta, RD: Siddipet, Medak (A.P.) 502277, India

Received on: 14-05-2011; Revised on: 15-06-2011; Accepted on:09-07-2011

ABSTRACT
The present research work discusses the development of UV-spectroscopic method for estimation of Naproxen. Simple, specific, accurate and cost effective
spectroscopic method has been developed for estimation of naproxen sodium in bulk as well as formulation. The optimum conditions for the analysis of the
drug were established. The maximum wavelength (λ max) was found to be 273 nm. The validation was performed as per ICH guidelines for linearity, accuracy,
precision, LOD and LOQ. The method shows high sensitivity with linearity in the range of 1-12 µg/ml. All calibration curves show a linear relationship between
the absorbance and concentration with coefficient of correlation 0.999. The regression of curve was Y = 0.016x + 0.001. The precision of method was found
to be good. The percentage recovery was found to be 100% ± SD. The optimized method showed good reproducibility and recovery with standard deviation <
1 % and percent relative standard deviation less than 2 %. Standard errors in case of recovery studies was satisfactorily low and allow estimation naproxen in
concentration range employed for this purpose in the assay of bulk drug and tablets. The sample solution was stable upto 36 hours. The proposed method will
be suitable for analysis of naproxen in bulk as well as pharmaceutical formulations in quality control purpose. It is thus concluded that the proposed method is
new, simple, cost-effective, safe, accurate, precise and environmental friendly.

Keywords: Naproxen, accuracy, sensitive, ICH guidelines

INTRODUCTION
Naproxen is NSAID agents which produces analgesia by interfering in produc- Construction of standard graph of naproxen
tion of prostaglandins. Chemically Naproxen is (+)-2-(6-methoxy-2-naph- Accurately weighed amount of Naproxen (100 mg) was transferred to a 100ml
thyl))-propionic acid 1 (Figure 1). It is available as white to slight yellow, volumetric flask. 50 mL of 7.2 phosphate buffer (containing 0.5%v\v of
odorless crystalline power having melting point in the range of 250 –256°C. It TWEEN 80) was added to dissolve the drug and volume was made up to 100 mL.
is only sparingly soluble in water, but soluble in methanol, ethanol and aceto- The resultant solution had the concentration of 1mg/ml which was labeled as
nitrile 2 . ‘Stock’. From this stock solution 10 ml was diluted to 100 mL with 7.2
phosphate buffer which has given the solution having the concentration of
It is official in British Pharmaco- 100µg/mL. Necessary dilutions were made by using this second solution to give
poeia. Several analytical techniques the different concentrations of Naproxen (1 to 12µg/mL) solutions.
like, spectrofluorimetric, HPLC,
RP–HPLC, spectrophotometric have The absorbance of above solutions was recorded at λ max (273nm) of the drug
been reported for assay of Naproxen 3- using double beam UV-Visible spectrophotometer. Standard graph was plotted
7
. However some of these methods between the concentration (on X-axis) and absorbance (on Y-axis).
are costlier and time consuming. To
overcome these difficulties spectro- Method Validation
photometric analysis serves to be the Various method of analysis of naproxen in bulk and pharmaceutical formula-
quickest, promising and reliable Figure 1: Chemical structure of tions (marketed and developed) was carried out as ICH guidelines Q2(R) 8-12.
method for routine analytical needs. Naproxen
Measurement of absorbance and calibration curve
The aim of the present study is to develop a new simple, rapid, reliable and The absorbance of solutions containing 6µg/ml was determined in UV range
precise UV spectrophotometric method for analysis of naproxen from tablet 200-800 nm using 7.2 phosphate buffer as blank. The λ max was found to be 273
formulation; method is based on measurement of UV absorbance of naproxen nm. At this wavelength maximum, calibration curve was drawn by plotting
in phosphate buffer pH 7.2. graph between absorbance and concentration. But from further literature and
experimental analysis it was found that, reproducible results can be obtained at
MATERIALS AND METHODS 278 nm.

Materials
Naproxen sodium was supplied by Ajanta Pharmaceuticals Ltd (Mumbai, In-
dia). All other chemicals were purchased from local vendor and used without
further purification. For preparation of analytical reagents and solutions Milli-
Q Pore water was used. Tablets of napoxen purchased from local market and
formulated were used for all relevant analysis.
Instrumentation
Drug concentrations in various tests was determined spectrophotometrically
(SL-164 Double beam UV spectrophotometer, Elico, India.) at 278 nm using
1 cm quartz match cells. For dilutions various micropipettes of volumes 10-
100 µl (Gene Pete Co.) were used. All weighing operations were done on
Schimadzu Digital Analytical Balance (Japan).
*Corresponding author.
Vinay Wamorkar
Department of Pharmaceutics,
Srikrupa Institute of Pharmaceutical Sciences,
Velkatta, RD: Siddipet,
Medak (A.P.) 502277, India
Linearity
The aliquots of concentrations ranging from 1-20 µg/ml were prepared in
triplicate, but linearity was found to be between 1-12 µg/ml. Statistical param-
eters like slope, intercept, coefficient of correlation, standard deviation and
relative standard deviation were determined.
Precision and accuracy
Precision is degree of repeatability of an analytical method under normal
operation conditions. The precision and accuracy were determined with stan-
dard quality control samples prepared in triplicate at different concentration
levels covering the entire linearity range. The precision of assay was deter-
mined by repeatability (intraday), intermediate precision (inter-day) and re-
ported as %RSD for a statistically significant number of replicate measure-
ments. The intermediate precision was studied by comparing the assay on
three different days and the results are documented as the standard deviation
and %RSD. Accuracy is the percentage of analyte recovered by assay from
known added amount. Data from nine determinations over three concentra-
tion levels covering the specified range were obtained.
Limit of Detection and Limit of Quantification
The limit of detection (LOD) is defined as the lowest concentration of an
analyte that an analytical process can reliably differentiate from back-ground
levels. In this study LOD and LOQ were based on the standard deviation of
response and the slope of corresponding curve using following equation:

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 Vinay Wamorkar et al. / Journal of Pharmacy Research 2011,4(8),2633-2635
LOD = 3.3 σ/ S Table 1: Linearity study of naproxen in phosphate buffer 7.2 at 278 nm
Where σ is standard deviation of Y-intercept and S is slope of calibration
curve. SL. No Concentration (µg/ml) Absorbance (278nm)

1 1 0.019
The limit of quantification (LOQ) is defined as the lowest concentration of 2 2 0.035
calibration curve that can be measured with an acceptable accuracy, precision 3 4 0.07
4 6 0.099
and variability. The value of LOQ was determined using following equation: 5 8 0.132
LOQ = = 10 σ/ S 6 10 0.169
7 12 0.202
Recovery study
Recovery of the analyte of interest from a given matrix can be used as a
measure of the accuracy or the bias of the method. The same range of concen-
trations, as employed in the linearity studies, was used. To study the accuracy,
precision and reproducibility of the proposed method and dosage forms, re-
covery experiments were carried out using the standard addition method.
These studies were performed by the addition of known amounts of pure
naproxen to the pre-analyzed tablet formulation and the mixtures were ana-
lyzed using the proposed techniques. After parallel analyses, the recovery
results were calculated using the related calibration equations.

Robustness
The evaluation of robustness was performed for system suitability to ensure
validity of analytical method. This was done by varying the, analyst, make of
chemical agents and solvents used.
Figure 3: Standard calibration curve of naproxen
Stability studies
The stability of naproxen in solution was studied by the UV method. Sample Table 2: Optical characteristics and precision
solutions were prepared in triplicate and stored at 4 and 25°C for 3 days.
Parameter Value
RESULTS AND DISCUSSION Absorption maxima 273 nm
In the start of the method development for this drug, different solvents were Beer’s law limit 0 – 12 µg/mL
tested such as water, methanol, 0.1N HCl, 0.1N NaOH and Phosphate buffer Coefficient of Correlation 0.999809
(pH7.2). For greater solubility and reproducible 0.5% v/v Tweens 80 was added Regression equation Y = 0.016 X + 0.001
Slope 0.016
and used for all further work. y intercept 0.001
% COV 0.011869
Naproxen is a UV-absorbing molecule with specific chromophores in the struc- Confidence limit (with 0.05 level) 0.00024
ture that absorb at a particular wavelength and this fact was successfully
employed for their quantitative determinations using the UV spectrophoto- Analytical method validation
metric method. Theλ ax of the drug for analysis was determined by taking scans The data was statistically validated by means of least square regression method.
of the drug sample solutions in the entire UV region. It was found to be that The detection and quantization limits were found to be 1.89 and 6.31. The
only one peak was observed in this method at the wavelength of 273 nm mean percentage drug estimated was 100.57 indicating the accuracy of the
(Figure 2). From scan it was confirmed that the addition of suitable surfac- proposed analytical method (Table 3).
tant increased solubility of drug.
Table 3: Result of pharmaceutical formulation analysis
Parameter Marketed Formulated
Sample Tablet

Label claim (mg) 250 250

Found (mg) 250.11 250.17
Drug content 100.5 101.85
±SD 0.212 0.210
%COV 0.090 0.096
SE 0.192 0.170

Mean standard deviation and standard error for naproxen was found to be 0.212
and 0.210 respectively. The low values of these statistical parameters validated
the method. The value of mean percentage recovery was 100.16 (Table 4).

Table 4: Results of recovery studies

Formulation Label claim (mg) Amount (mg/ml) % Recovery ±SD %COV
Taken Added

Marketed Tablet 250 5 2 100.03 ±0.12 0.211

10 4 100.12 ±0.37 0.203
15 6 101.33 ±0.55 0.321
Formulated Tablet 250 5 2 101.23 ±0.27 0.322

Figure 2: UV-scan of naproxen in phosphate buffer with (A) and with- 10 4 99.26 ±0.45 0.431
15 6
out Tweens 80 (B)
Calibration curves % Recovery is mean of three estimations
Calibration curve data were constructed in the range of the expected concentra- SD: Standard deviation
tions of 1µg/mL to 12µg/mL. Beer’s law was obeyed over this concentration COV: Coefficient of variance
range. The regression equation was found to be Y = 0.016x + 0.001. The This fact, together with satisfactory low values of statistical parameters (Table
correlation coefficient (r) of the standard curve was found to be greater than 5), further validated the method. There was no interference of excipients in the
0.999. Linearity range and calibration curve is presented in Table 1 and Figure estimation. The proposed method can be successfully employed in the routine
3. Further statistical evaluation was done and data is as presented in Table 2. analysis of naproxen containing dosage forms.

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Table 5: Validation data of UV method for naproxen REFERENCES
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Source of support: Nil, Conflict of interest: None Declared

101.24 ±0.17 0.377

Journal of Pharmacy Research Vol.4.Issue 8. August 2011 2633-2635