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Development and Validation of a LC-MS/MS Method for the Simultaneous Estimation of Amlodipine and Valsartan in Human Plasma: Application to a Bioequivalence Study.

Jangala H, Vats P, Khuroo AH, Monif T - Sci Pharm (2014)

Bottom Line: The assay was found to be linear over the range of 0.302-20.725 ng/mL for amlodipine and 6.062-18060.792 ng/mL for valsartan.The method was successfully applied for the bioequivalence study of amlodipine and valsartan after oral administration of a fixed dose of the combination.Additionally, as required by the current regulatory bodies, incurred sample reanalysis was performed and found to be acceptable.

View Article: PubMed Central - PubMed

Affiliation: Clinical Pharmacology and Pharmacokinetics, Ranbaxy Research Laboratories, Gurgaon, India.

ABSTRACT
A reliable, simple, and robust liquid chromatography-tandem mass spectro-metric (LC-MS/MS) method has been developed and validated that employs solid-phase extraction for the simultaneous estimation of amlodipine and valsartan in human K3EDTA plasma using amlodipine-d4 and valsartan-d9 as internal standards. Chromatographic separation of amlodipine and valsartan was achieved on the Luna C18 (2)100A (150 × 4.6 mm, 5 μm) column using acetonitrile: 5 mM ammonium formate solution (80:20, v/v) as the mobile phase at a flow rate of 0.8 mL/min in isocratic mode. Quantification was achieved using an electrospray ion interface operating in positive mode, under multiple reaction monitoring (MRM) conditions. The assay was found to be linear over the range of 0.302-20.725 ng/mL for amlodipine and 6.062-18060.792 ng/mL for valsartan. The method has shown good reproducibility, as intra- and interday precisions were within 10% and accuracies were within 8% of nominal values for both analytes. The method was successfully applied for the bioequivalence study of amlodipine and valsartan after oral administration of a fixed dose of the combination. Additionally, as required by the current regulatory bodies, incurred sample reanalysis was performed and found to be acceptable.

No MeSH data available.


Related in: MedlinePlus

Representative chromatograms of amlodipine and valsartan: 1. double blank sample; 2. LOQ
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Figure 2: Representative chromatograms of amlodipine and valsartan: 1. double blank sample; 2. LOQ

Mentions: There was no significant interference observed at the retention times of the analytes and internal standards assessed by calculating % interference derived from the processed blank plasma sample against the mean peak area of the LOQ samples. The typical chromatograms of the double blank and LOQ in human plasma are shown in Figure 2. The limit of quantification was 0.302 ng/mL and 6.062 ng/mL for amlodipine and valsartan, respectively. The precision and accuracy at the LOQ concentration for amlodipine were 4.5% and 99.3% and for valsartan, 8.0% and 103.4%, respectively. The mean signal-to-noise ratios of the LOQ samples with respect to the blank matrix samples were 140.0 and 35.5 for amlodipine and valsartan, respectively. The retention times of amlodipine and valsartan under the optimized chromatographic conditions were 1.7 and 2.2 minutes, respectively.


Development and Validation of a LC-MS/MS Method for the Simultaneous Estimation of Amlodipine and Valsartan in Human Plasma: Application to a Bioequivalence Study.

Jangala H, Vats P, Khuroo AH, Monif T - Sci Pharm (2014)

Representative chromatograms of amlodipine and valsartan: 1. double blank sample; 2. LOQ
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4318187&req=5

Figure 2: Representative chromatograms of amlodipine and valsartan: 1. double blank sample; 2. LOQ
Mentions: There was no significant interference observed at the retention times of the analytes and internal standards assessed by calculating % interference derived from the processed blank plasma sample against the mean peak area of the LOQ samples. The typical chromatograms of the double blank and LOQ in human plasma are shown in Figure 2. The limit of quantification was 0.302 ng/mL and 6.062 ng/mL for amlodipine and valsartan, respectively. The precision and accuracy at the LOQ concentration for amlodipine were 4.5% and 99.3% and for valsartan, 8.0% and 103.4%, respectively. The mean signal-to-noise ratios of the LOQ samples with respect to the blank matrix samples were 140.0 and 35.5 for amlodipine and valsartan, respectively. The retention times of amlodipine and valsartan under the optimized chromatographic conditions were 1.7 and 2.2 minutes, respectively.

Bottom Line: The assay was found to be linear over the range of 0.302-20.725 ng/mL for amlodipine and 6.062-18060.792 ng/mL for valsartan.The method was successfully applied for the bioequivalence study of amlodipine and valsartan after oral administration of a fixed dose of the combination.Additionally, as required by the current regulatory bodies, incurred sample reanalysis was performed and found to be acceptable.

View Article: PubMed Central - PubMed

Affiliation: Clinical Pharmacology and Pharmacokinetics, Ranbaxy Research Laboratories, Gurgaon, India.

ABSTRACT
A reliable, simple, and robust liquid chromatography-tandem mass spectro-metric (LC-MS/MS) method has been developed and validated that employs solid-phase extraction for the simultaneous estimation of amlodipine and valsartan in human K3EDTA plasma using amlodipine-d4 and valsartan-d9 as internal standards. Chromatographic separation of amlodipine and valsartan was achieved on the Luna C18 (2)100A (150 × 4.6 mm, 5 μm) column using acetonitrile: 5 mM ammonium formate solution (80:20, v/v) as the mobile phase at a flow rate of 0.8 mL/min in isocratic mode. Quantification was achieved using an electrospray ion interface operating in positive mode, under multiple reaction monitoring (MRM) conditions. The assay was found to be linear over the range of 0.302-20.725 ng/mL for amlodipine and 6.062-18060.792 ng/mL for valsartan. The method has shown good reproducibility, as intra- and interday precisions were within 10% and accuracies were within 8% of nominal values for both analytes. The method was successfully applied for the bioequivalence study of amlodipine and valsartan after oral administration of a fixed dose of the combination. Additionally, as required by the current regulatory bodies, incurred sample reanalysis was performed and found to be acceptable.

No MeSH data available.


Related in: MedlinePlus