INTRODUCTION: Analytical chemistry, like other areas of chemistry and science, has gone through
drastic changes and growth. Analytical chemistry may defined as the “Science and art of
determining the composition of materials in terms of the elements or compounds
contained”. In analytical chemistry it is of prime importance to gain information about the
qualitative and quantitative composition of substances and chemical species, that is to find
out what a substance is composed of and exactly how much .
Analytical method is a specific application of a technique to solve an analytical
problem. The use of instrumentation is an exciting and fascinating part of chemical analysis
that interacts with all areas of chemistry and with many other areas of pure and applied
science. Analytical instrumentation plays an important role in the production and
evaluation of new products and in the protection of consumers and the environment. This
instrumentation provides the lower detection limits required to assure safe foods, drugs and
water. The manufacture of materials, whose composition must be known precisely such as
substances used in integrated circuit chips, is monitored by analytical instruments.
Instrumental or physicochemical methods are based on the theory of relations
between the content and the corresponding physicochemical and physical properties of the
chemical system being analyzed. Changes in the system properties are either detected or
recorded through the measurement of current, electrode potential, electrical conductivity,
optical density, refractive index etc. with suitable and sensitive instruments. In instrumental
analysis physical property of substance is measured to determine its chemical composition.
Measurements of physical properties of analyte such as conductivity, electrode
potential, light absorption or emission, mass to charge ratio, and fluorescence, began to be
used for quantitative analysis of variety of inorganic and biochemical analyses. Highly
efficient chromatographic and electrophoretic techniques began to replace distillation,
extraction, and precipitation for the separation of components of complex mixtures prior to
their qualitative or quantitative determination. AIM: To develop and validate the method for simultaneous estimation of Naproxen and
Esomeprazole magnesium by RP-HPLC. OBJECTIVES: On literature survey it was found that Naproxen and Esomeprazole magnesium is
estimated by HPLC and UV Spectrophotometric methods, in combination with other drugs
in tablet and bulk dosage form.
However no method could be found for simultaneous estimation of Naproxen and
Esomeprazole magnesium, and also no method was available for such estimation in the
pharmacopoeia. In view of the need for a suitable method for routine analysis of Naproxen
and Esomeprazole magnesium in formulations, attempts are being made to develop simple,
precise and accurate analytical methods for simultaneous estimation of Naproxen and
Esomeprazole magnesium and extend it for their determination in formulations.
The utility of the developed methods to determine the content of both drugs in
commercial tablet is also demonstrated. Validation of the method was done in accordance
with USP and ICH guidelines for the assay of active ingredients. The methods were
validated for parameters like accuracy, linearity, precision, specificity, ruggedness,
robustness, and system suitability. These methods provide means to separate the individual
components of a mixture and simultaneously characterize and quantify the components.
These proposed methods are suitable for the pharmaceutical analysis in analytical
laboratories.
The Chromatographic methods proposed in this presume that there is a linear
relationship between absorbance and component concentration. These methods have a
calibration step followed by the prediction step, in which the results of the calibration step
are used to estimate the component concentration from an unknown sample spectrum. The
Chromatographic methods have many of full spectrum advantages. These methods are
known to provide additional advantages that calibration can be performed by ignoring the
concentration of all other components except the analyte of interest. These methods have been successfully applied to the quantitative analysis in spectrophotometric,
chromatographic and electrochemical data.
In summary, the primary objective of proposed work is to:-
1. Develop new, simple, sensitive, accurate, and economical analytical methods for the
simultaneous estimation of Naproxen and Esomeprazole magnesium.
2. Validate the proposed methods in accordance with USP and ICH guidelines for the
intended analytical application i.e., to apply the proposed method for analysis of these drugs in their combined dosage form. RESULT AND DISCUSSION: The objective of the proposed work was method development for the simultaneous estimation of Naproxen and Esomeprazole magnesium in tablets by RP-HPLC and to validate the developed method according to USP and ICH guidelines and applying the same for use in the quality control samples in pharmaceutical industry.
As there is no official method for the simultaneous estimation of Naproxen and Esomeprazole magnesium in this selective combination, so we tried to develop a method
by which we can quantify the amount of drug present in the given sample.
In RP-HPLC method, the conditions were optimized to obtain an adequate separation of eluted compounds. Initially, various mobile phase compositions were tried, to
separate titled ingredients. Mobile phase and flow rate selection was based on peak parameters (height, tailing, theoretical plates, capacity or symmetry factor), run time and resolution. The system with pH7.3 Phosphate Buffer: ACN: Water (50:35:15) at flow rate of 1.0 ml/min
was found to be quite robust.
The optimum wavelength for detection was 302 nm at which better detector response for both the drugs was obtained. The average retention times for Naproxen and Esomeprazole magnesium was found to be 3.397 and 8.146 min, respectively. According toUnited States Pharmacopeia, system suitability tests are an integral part of chromatographic method. They are used to verify the reproducibility of the chromatographic system. To ascertain its effectiveness, system suitability tests were carried out on freshly prepared stock solutions. The calibration was linear in various concentration range with correlation.
The low values of RSD indicate that the method was precise and accurate. The mean recoveries were found in the range of 98 – 102 %. System precision is evaluated by injecting 6 injections of standard solution and low value of % RSD shows that system is precise. Precision for method is evaluated by analyzing a sample of homogenous batch six times and the low % RSD value shows the method is precise.
Method robustness was evaluated by alteration of flow rate (±0.2 mL), Wavelength (± 2 nm), Mobile phase Organic Content (±5%) and it was found robust as % RSD was below 2.0%.
Ruggedness of the proposed method was determined by analysis of aliquots from homogeneous slot in different laboratories, by different analysts, different column, different
system using similar environmental conditions, the % R.S.D. reported was found to be less than 2 %. The proposed method was validated in accordance with ICH parameters and the
applied for analysis of the same in marketed formulations.
Both sample solution and standard solution are stable at 25°C for 24 hrs. as the % difference in the RSD was found to be less than 2.0%.
Finally, it can be concluded that the assay values of formulation were the same as mentioned in the label claim with the RSD of ≤ 2.0%.
The proposed method was found to be accurate, precise, reproducible and stable, and can be successfully applied for the routine analysis of both the drugs in combined
tablet dosage forms. CONCLUSION: An efficient high performance liquid chromatographic method was developed and
validated for the simultaneous estimation of Naproxen and Esomeprazole magnesium. In RP-HPLC method, the conditions were optimized to obtain an adequate separation of
eluted compounds. Initially, various mobile phase compositions were tried, to separate titled ingredients. Mobile phase and flow rate selection was based on peak parameters (height, tailing, theoretical plates, capacity or symmetry factor), run time and resolution.
The system with pH 7.3 Phosphate buffer: ACN: Water at flow rate of 1.0 mL/min
was
found to be quite robust.
The low values of RSD indicate that the method was precise and accurate. The
mean recoveries were found in the range of 98 – 102 %. System precision is evaluated by
injecting 6 injections of standard solution and low value of % RSD shows that system is
precise. Precision for method is evaluated by analysing a sample of homogenous batch six
times and the low % RSD value shows the method precise
