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Validated Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Azelnidipine and Olmesartan in Their Combined Dosage Form.

Patel JK, Patel NK - Sci Pharm (2014)

Bottom Line: The retention times for Azelnidipine and Olmesartan were about 8.56 and 3.04 min, respectively.Calibration curves were linear in the ranges of 2-48 μg/mL for Azelnidipine and 2.5-60 μg/mL for Olmesartan with correlation coefficients >0.990.The proposed method proved to be selective and stability-indicating by the resolution of the two analytes from the forced degradation (hydrolysis, oxidation, and photolysis) products.

View Article: PubMed Central - PubMed

Affiliation: Nootan Pharmacy College, S.P. Sahkar Vidhyadham, Kamana Crossing, Visnagar 384315, Mehsana, Gujarat, India.

ABSTRACT
A simple, rapid, and highly selective RP-HPLC method was developed for the simultaneous determination of Azelnidipine (AZL) and Olmesartan (OLM) drug substances in the fixed dosage strength of 16 mg and 20 mg, respectively. Effective chromatographic separation was achieved using a Hypersil GOLD C18 column (150 mm × 4.6 mm internal diameter, 5 µm particle size) with a mobile phase composed of methanol, acetonitrile, and water in the ratio of 40:40:20 (by volume). The mobile phase was pumped using a gradient HPLC system at a flow rate of 0.5 mL/min, and quantification of the analytes was based on measuring their peak areas at 260 nm. The retention times for Azelnidipine and Olmesartan were about 8.56 and 3.04 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Calibration curves were linear in the ranges of 2-48 μg/mL for Azelnidipine and 2.5-60 μg/mL for Olmesartan with correlation coefficients >0.990. The proposed method proved to be selective and stability-indicating by the resolution of the two analytes from the forced degradation (hydrolysis, oxidation, and photolysis) products. The validated HPLC method was successfully applied to the analysis of AZL and OLM in their combined dosage form.

No MeSH data available.


Related in: MedlinePlus

Placebo chromatogram
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Figure 1: Placebo chromatogram

Mentions: For the study, 16 µg/ml of Azelnidipine and 20 µg/ml of Olmesartan solution were prepared for the entire standard. Different columns like the Hypersil GOLD C18 column (150 mm × 4.6 mm internal diameter, 5 µm particle size), Kromasil 100 C8 column (50 mm × 4.6 mm internal diameter, 5 µm particle size), and ACE 5 C18 column (150 mm × 4.6 mm internal diameter, 5 µm particle size) were tried for method development. The Hypersil gold column gave better results compared to the other column. In almost every system (with changes in the mobile phase) studied, Azelnidipine and Olmesartan showed retention times greater than 8.5 min and 3.0 min, respectively. Other mobile phase combinations resulted in > 8.5 min and 3.0 min, where the separation of AZL and OLM from each other and from excipients/degradation products was worse than the optimal conditions. The optimized mobile phase was composed of methanol, acetonitrile, and water in the ratio of 40:40:20 v/v/v. It was not required to change the pH of the mobile phase, as both drugs had well-resolved peaks in the optimized mobile phase. Figure 1 shows a typical chromatogram of the placebo at the optimized conditions. Figure 2 also shows a typical HPLC chromatogram of the freshly prepared mixture of AZL and OLM using the optimized conditions.


Validated Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Azelnidipine and Olmesartan in Their Combined Dosage Form.

Patel JK, Patel NK - Sci Pharm (2014)

Placebo chromatogram
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4318177&req=5

Figure 1: Placebo chromatogram
Mentions: For the study, 16 µg/ml of Azelnidipine and 20 µg/ml of Olmesartan solution were prepared for the entire standard. Different columns like the Hypersil GOLD C18 column (150 mm × 4.6 mm internal diameter, 5 µm particle size), Kromasil 100 C8 column (50 mm × 4.6 mm internal diameter, 5 µm particle size), and ACE 5 C18 column (150 mm × 4.6 mm internal diameter, 5 µm particle size) were tried for method development. The Hypersil gold column gave better results compared to the other column. In almost every system (with changes in the mobile phase) studied, Azelnidipine and Olmesartan showed retention times greater than 8.5 min and 3.0 min, respectively. Other mobile phase combinations resulted in > 8.5 min and 3.0 min, where the separation of AZL and OLM from each other and from excipients/degradation products was worse than the optimal conditions. The optimized mobile phase was composed of methanol, acetonitrile, and water in the ratio of 40:40:20 v/v/v. It was not required to change the pH of the mobile phase, as both drugs had well-resolved peaks in the optimized mobile phase. Figure 1 shows a typical chromatogram of the placebo at the optimized conditions. Figure 2 also shows a typical HPLC chromatogram of the freshly prepared mixture of AZL and OLM using the optimized conditions.

Bottom Line: The retention times for Azelnidipine and Olmesartan were about 8.56 and 3.04 min, respectively.Calibration curves were linear in the ranges of 2-48 μg/mL for Azelnidipine and 2.5-60 μg/mL for Olmesartan with correlation coefficients >0.990.The proposed method proved to be selective and stability-indicating by the resolution of the two analytes from the forced degradation (hydrolysis, oxidation, and photolysis) products.

View Article: PubMed Central - PubMed

Affiliation: Nootan Pharmacy College, S.P. Sahkar Vidhyadham, Kamana Crossing, Visnagar 384315, Mehsana, Gujarat, India.

ABSTRACT
A simple, rapid, and highly selective RP-HPLC method was developed for the simultaneous determination of Azelnidipine (AZL) and Olmesartan (OLM) drug substances in the fixed dosage strength of 16 mg and 20 mg, respectively. Effective chromatographic separation was achieved using a Hypersil GOLD C18 column (150 mm × 4.6 mm internal diameter, 5 µm particle size) with a mobile phase composed of methanol, acetonitrile, and water in the ratio of 40:40:20 (by volume). The mobile phase was pumped using a gradient HPLC system at a flow rate of 0.5 mL/min, and quantification of the analytes was based on measuring their peak areas at 260 nm. The retention times for Azelnidipine and Olmesartan were about 8.56 and 3.04 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Calibration curves were linear in the ranges of 2-48 μg/mL for Azelnidipine and 2.5-60 μg/mL for Olmesartan with correlation coefficients >0.990. The proposed method proved to be selective and stability-indicating by the resolution of the two analytes from the forced degradation (hydrolysis, oxidation, and photolysis) products. The validated HPLC method was successfully applied to the analysis of AZL and OLM in their combined dosage form.

No MeSH data available.


Related in: MedlinePlus