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Development and Validation of HPTLC Method for the Estimation of Almotriptan Malate in Tablet Dosage Form.

Suneetha A, Syamasundar B - Indian J Pharm Sci (2010)

Bottom Line: The method was validated for linearity, accuracy, precision and robustness.The calibration plot was linear over the range of 100-700 ng/band for almotriptan malate.The method was successfully applied to the analysis of drug in a pharmaceutical dosage form.

View Article: PubMed Central - PubMed

Affiliation: Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur-522 002, India.

ABSTRACT
A new, simple, precise and accurate high performance thin layer chromatographic method has been proposed for the determination of almotriptan malate in a tablet dosage form. The drug was separated on aluminum plates precoated with silica gel 60 GF(254) with butanol:acetic acid:water (3:1:1) was used as mobilephase. Quantitative analysis was performed by densitometric scanning at 300 nm. The method was validated for linearity, accuracy, precision and robustness. The calibration plot was linear over the range of 100-700 ng/band for almotriptan malate. The method was successfully applied to the analysis of drug in a pharmaceutical dosage form.

No MeSH data available.


Densitogram obtained from a sample solution of almotriptan malate
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Figure 2: Densitogram obtained from a sample solution of almotriptan malate

Mentions: For optimization of method, different mobile phase compositions were employed to achieve good separation. The method development was initiated by using different proportions of mobile phase consisting variety of solvents like: toluene:methanol:ethylacetate, dichloromethane:methanol, butanol:aceticacid:water, toluene:methanol:acetone, toluene:methanol:ethylacetate:aceticacid, hexane:ethylacetate. Of these the mixture butanol-acetic acid-water 3:1:1 (v/v) was found to be suitable for the studies. The RF value of almotriptan malate was 0.53±0.01. The proposed HPTLC method was validated in terms of linearity, precision, accuracy, specificity and robustness. The calibration plot was found to be linear over the range 100–700 ng/band for almotriptan malate, with a correlation coefficient of 0.9994±0.0002. The LOD and LOQ were found to be 28.19 and 93.99 ng/band, respectively. The values of percent relative standard deviations were found to be 0.23 and 0.51 for Intraday and inter day precision studies, respectively which indicate that the method is precise. The method was also evaluated by assay of commercially available tablets (Axert) containing almotriptan malate. The resulting densitogram for a sample solution of almotriptan malate is presented in fig. 2] indicating a concentration of 700 ng/band. Six replicate analyses were performed on accurately weighed amount of the tablets (Table 1). The percent assay was found to be 99.36±0.522 for almotriptan malate. To study the accuracy of the method, recovery studies were performed. For almotriptan malate, recovery ranged from 99.54 to 101.1% with values of percent RSD ranging from 0.21 to 0.61 indicating that the proposed HPTLC method is highly accurate (Table 2). To confirm the specificity of the proposed method, the solution of formulation was spotted on TLC plate, developed and scanned. It was observed that the excipients present in the formulation did not interfere with the sample peak. Study of the robustness of the method revealed that the peak areas were unaffected (RSD < 2%) by small changes in composition and volume of mobile phase indicating appreciable robustness of the method. The method validation parameters are presented in (Table 3).


Development and Validation of HPTLC Method for the Estimation of Almotriptan Malate in Tablet Dosage Form.

Suneetha A, Syamasundar B - Indian J Pharm Sci (2010)

Densitogram obtained from a sample solution of almotriptan malate
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3116310&req=5

Figure 2: Densitogram obtained from a sample solution of almotriptan malate
Mentions: For optimization of method, different mobile phase compositions were employed to achieve good separation. The method development was initiated by using different proportions of mobile phase consisting variety of solvents like: toluene:methanol:ethylacetate, dichloromethane:methanol, butanol:aceticacid:water, toluene:methanol:acetone, toluene:methanol:ethylacetate:aceticacid, hexane:ethylacetate. Of these the mixture butanol-acetic acid-water 3:1:1 (v/v) was found to be suitable for the studies. The RF value of almotriptan malate was 0.53±0.01. The proposed HPTLC method was validated in terms of linearity, precision, accuracy, specificity and robustness. The calibration plot was found to be linear over the range 100–700 ng/band for almotriptan malate, with a correlation coefficient of 0.9994±0.0002. The LOD and LOQ were found to be 28.19 and 93.99 ng/band, respectively. The values of percent relative standard deviations were found to be 0.23 and 0.51 for Intraday and inter day precision studies, respectively which indicate that the method is precise. The method was also evaluated by assay of commercially available tablets (Axert) containing almotriptan malate. The resulting densitogram for a sample solution of almotriptan malate is presented in fig. 2] indicating a concentration of 700 ng/band. Six replicate analyses were performed on accurately weighed amount of the tablets (Table 1). The percent assay was found to be 99.36±0.522 for almotriptan malate. To study the accuracy of the method, recovery studies were performed. For almotriptan malate, recovery ranged from 99.54 to 101.1% with values of percent RSD ranging from 0.21 to 0.61 indicating that the proposed HPTLC method is highly accurate (Table 2). To confirm the specificity of the proposed method, the solution of formulation was spotted on TLC plate, developed and scanned. It was observed that the excipients present in the formulation did not interfere with the sample peak. Study of the robustness of the method revealed that the peak areas were unaffected (RSD < 2%) by small changes in composition and volume of mobile phase indicating appreciable robustness of the method. The method validation parameters are presented in (Table 3).

Bottom Line: The method was validated for linearity, accuracy, precision and robustness.The calibration plot was linear over the range of 100-700 ng/band for almotriptan malate.The method was successfully applied to the analysis of drug in a pharmaceutical dosage form.

View Article: PubMed Central - PubMed

Affiliation: Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur-522 002, India.

ABSTRACT
A new, simple, precise and accurate high performance thin layer chromatographic method has been proposed for the determination of almotriptan malate in a tablet dosage form. The drug was separated on aluminum plates precoated with silica gel 60 GF(254) with butanol:acetic acid:water (3:1:1) was used as mobilephase. Quantitative analysis was performed by densitometric scanning at 300 nm. The method was validated for linearity, accuracy, precision and robustness. The calibration plot was linear over the range of 100-700 ng/band for almotriptan malate. The method was successfully applied to the analysis of drug in a pharmaceutical dosage form.

No MeSH data available.