Tags

Type your tag names separated by a space and hit enter

HPLC method for determination of DRF-4367 in rat plasma: validation and its application to pharmacokinetics in Wistar rats.
Biomed Chromatogr. 2004 Oct; 18(8):576-80.BC

Abstract

A specific, accurate, precise and reproducible high-performance liquid chromatography (HPLC) method was developed for the estimation of DRF-4367, a novel cyclooxygenase-2 inhibitor in rat plasma. The assay procedure involved simple liquid/liquid extraction of DRF-4367 and internal standard (IS, celecoxib) from plasma into dichloromethane. The organic layer was separated and evaporated under a gentle stream of nitrogen at 40 degrees C. The residue was reconstituted in the mobile phase and injected onto a Kromasil KR 100-5C(18) column (4.6 x 250 mm, 5 microm). The mobile phase consisting of 0.01 M potassium dihydrogen ortho-phosphate (pH 3.2) and acetonitrile (40:60, v/v) was used at a flow rate of 1.0 mL/min. The eluate was monitored using an UV detector set at 247 nm. The ratio of peak area of analyte to IS was used for quantification of plasma samples. Nominal retention times of DRF-4367 and IS were 6.6 and 11.2 min, respectively. The standard curve for DRF-4367 was linear (r(2) > 0.999) in the concentration range 0.1-20 micro g/mL. Absolute recovery was >86% from rat plasma for both analyte and IS. The lower limit of quantification of DRF-4367 was 0.1 micro g/mL. The inter- and intra-day precisions in the measurement of quality control samples, 0.1, 0.3, 8.0 and 15.0 microg/mL, were in the range 6.93-9.34% relative standard deviation (RSD) and 0.48-6.59% RSD, respectively. Accuracy in the measurement of QC samples was in the range 91.24-109.36% of the nominal values. Analyte and IS were stable in the battery of stability studies, viz. benchtop, autosampler and freeze-thaw cycles. Stability of DRF-4367 was established for 1 month at -80 degrees C. The application of the assay to a pharmacokinetic study in rats is described.

Authors+Show Affiliations

Drug Metabolism and Pharmacokinetics, Discovery Research, Dr Reddy's Laboratories Ltd, Miyapur, Hyderabad-500 049, India.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

15386513

Citation

Mullangi, Ramesh, et al. "HPLC Method for Determination of DRF-4367 in Rat Plasma: Validation and Its Application to Pharmacokinetics in Wistar Rats." Biomedical Chromatography : BMC, vol. 18, no. 8, 2004, pp. 576-80.
Mullangi R, Kallem RR, Bhamidipati RK, et al. HPLC method for determination of DRF-4367 in rat plasma: validation and its application to pharmacokinetics in Wistar rats. Biomed Chromatogr. 2004;18(8):576-80.
Mullangi, R., Kallem, R. R., Bhamidipati, R. K., Mamidi, R. N., & Srinivas, N. R. (2004). HPLC method for determination of DRF-4367 in rat plasma: validation and its application to pharmacokinetics in Wistar rats. Biomedical Chromatography : BMC, 18(8), 576-80.
Mullangi R, et al. HPLC Method for Determination of DRF-4367 in Rat Plasma: Validation and Its Application to Pharmacokinetics in Wistar Rats. Biomed Chromatogr. 2004;18(8):576-80. PubMed PMID: 15386513.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - HPLC method for determination of DRF-4367 in rat plasma: validation and its application to pharmacokinetics in Wistar rats. AU - Mullangi,Ramesh, AU - Kallem,Raja Reddy, AU - Bhamidipati,Ravi Kanth, AU - Mamidi,Rao N V S, AU - Srinivas,Nuggehally R, PY - 2004/9/24/pubmed PY - 2005/2/11/medline PY - 2004/9/24/entrez SP - 576 EP - 80 JF - Biomedical chromatography : BMC JO - Biomed Chromatogr VL - 18 IS - 8 N2 - A specific, accurate, precise and reproducible high-performance liquid chromatography (HPLC) method was developed for the estimation of DRF-4367, a novel cyclooxygenase-2 inhibitor in rat plasma. The assay procedure involved simple liquid/liquid extraction of DRF-4367 and internal standard (IS, celecoxib) from plasma into dichloromethane. The organic layer was separated and evaporated under a gentle stream of nitrogen at 40 degrees C. The residue was reconstituted in the mobile phase and injected onto a Kromasil KR 100-5C(18) column (4.6 x 250 mm, 5 microm). The mobile phase consisting of 0.01 M potassium dihydrogen ortho-phosphate (pH 3.2) and acetonitrile (40:60, v/v) was used at a flow rate of 1.0 mL/min. The eluate was monitored using an UV detector set at 247 nm. The ratio of peak area of analyte to IS was used for quantification of plasma samples. Nominal retention times of DRF-4367 and IS were 6.6 and 11.2 min, respectively. The standard curve for DRF-4367 was linear (r(2) > 0.999) in the concentration range 0.1-20 micro g/mL. Absolute recovery was >86% from rat plasma for both analyte and IS. The lower limit of quantification of DRF-4367 was 0.1 micro g/mL. The inter- and intra-day precisions in the measurement of quality control samples, 0.1, 0.3, 8.0 and 15.0 microg/mL, were in the range 6.93-9.34% relative standard deviation (RSD) and 0.48-6.59% RSD, respectively. Accuracy in the measurement of QC samples was in the range 91.24-109.36% of the nominal values. Analyte and IS were stable in the battery of stability studies, viz. benchtop, autosampler and freeze-thaw cycles. Stability of DRF-4367 was established for 1 month at -80 degrees C. The application of the assay to a pharmacokinetic study in rats is described. SN - 0269-3879 UR - https://www.unboundmedicine.com/medline/citation/15386513/HPLC_method_for_determination_of_DRF_4367_in_rat_plasma:_validation_and_its_application_to_pharmacokinetics_in_Wistar_rats_ L2 - https://doi.org/10.1002/bmc.359 DB - PRIME DP - Unbound Medicine ER -