You are hereDevelopment and Validation of HPTLC Method for Simultaneous Estimation of Atorvastatin Calcium and Olmesartan Medoxomil in Tablet Dosage Form

Development and Validation of HPTLC Method for Simultaneous Estimation of Atorvastatin Calcium and Olmesartan Medoxomil in Tablet Dosage Form

6) Robustness and Ruggedness:
There were no significant difference between results obtained by applying the analytical condition established for the method and those obtained in experiments in which some of the conditions were varied slightly. Thus the method was shown to be robust to changes in acetonitrile proportion from 12-18 %. Plates were developed 5 min after spotting and scanned 15 min after development. The ruggedness of the method was checked by using different analysts and days. The relative standard deviation of the results obtained by different analysts using instruments was <2.0%.

7) Solution stability:
To check the stability of the drug by use of the proposed method, freshly prepared solutions of analytes were applied to the plates and developed after intervals of 2 h, 6 h and 12 h. Decomposition of the drugs were not observed during chromatogram development and no change in the peak area of the drugs were observed during solution stability studies.

8) Assay:
The proposed method was also evaluated by the assay of test sample of commercially availabletablets of AT and OLM. The % assay (Mean ± S.D) was found to be 99.89 ± 0.14 for AT and102.2 ± 0.11 for OLM

The mobile phase consisting of acetonitrile: chloroform: methanol: 10% GAA (7:2:1.5:0.1, v/v/v/v) gave Rf value of 0.50±0.01 and 0.76±0.02 for AT and OLM, respectively. The linear regression data (n=5, Table 1) showed a good linear relationship over a concentration range of 200-800 ng/spot for AT and 400-1600 ng/spot for OLM, respectively. The limit of detection and limit of quantification for AT was found to be 178.23 and 540.11 ng/spot and for OLM 40.1 and 121.51ng/spot, respectively.  The intra-day and inter-day coefficients of variation were less than 2 for both AT and OLM. Repeatability of sample application was assessed by spotting 5µl of drug solution 5 times on a TLC plate followed by development of plate and recording the peak area for 5 spots. The %RSD for peak area values of AT and OLM were found to be 1.09 and 1.06, respectively. To confirm the specificity of the proposed method, the solution of the formulation was spotted on the TLC plate, developed and scanned. It was observed that the excipients present in the formulation did not interfere with the peaks of drugs. Multiple recovery study was carried out for accuracy parameter. % recovery was found to be within the limit as listed in Table 2. The assay value for marketed formulation was found to be within the limits as listed in Table 3.

The developed HPTLC technique is simple, precise, specific and accurate and the statistical analysis proved that method is reproducible and selective for the analysis of olmesartan medoxomil and atorvastatin calcium in bulk drug and tablet formulation.

The authors wish to express their gratitude to Sun Pharmaceutical Ltd. Baroda (India), for providing gift sample of AT and OLM. The authors are also thankful to the Principal and Management, Shri Sarvajanik Pharmacy College for providing necessary facilities.

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