Quantitative determination of 21‐hydroxy‐deflazacort in human plasma using gradient semi‐microbore liquid chromatography

Reynolds, Donald L.; Burmaster, Steve; Eichmeier, Larry S.

doi:10.1002/bmc.1130080507

Cited by 9 publications

(4 citation statements)

References 3 publications

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“…A 7mL blood sample was collected in heparinized plasma pre-dose, and at 0.5, 1, 1.5,2, 3,4,6,8,10,12,16,20, and 24 h post-dose. Plasma was separated by centrifugation and immediately frozen until analysis.…”

Section: Sampling Schemementioning

confidence: 99%

An Investigation of the Dose Proportionality of Deflazacort Pharmacokinetics

Rao¹,

Bhargava²,

Reynolds³

et al. 1996

Biopharm. Drug Dispos.

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Section: Sampling Schemementioning

confidence: 99%

An Investigation of the Dose Proportionality of Deflazacort Pharmacokinetics

Rao¹,

Bhargava²,

Reynolds³

et al. 1996

Biopharm. Drug Dispos.

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“…Deflazacort is employed in the treatment of rheumatoid arthritis, Ducchene dystrophy, systemic lupus erithematosus, uveitis and transplantation. 1 Although several method have been reported for the determination of 21-OH-DFZ in human plasma, all using high-performance liquid chromatographic (HPLC) separation and UV detection, 2 -6 only the method proposed by Reynolds et al 5 has the sensitivity required for pharmacokinetic studies, with low administration doses. The minimum quantification limit is 1 ng ml 1 .…”

Section: Introductionmentioning

confidence: 99%

Determination of 21-hydroxydeflazacort in human plasma by high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry. Application to bioequivalence study

Ifa

Moraes

et al. 2000

J. Mass Spectrom.

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A liquid chromatographic atmospheric pressure chemical ionization tandem mass spectrometric method is described for the determination of 21‐hydroxydeflazacort in human plasma using dexamethasone 21‐acetate as an internal standard. The procedure requires a single diethyl ether extraction. After evaporation of the solvent under a nitrogen flow, the analytes are reconstituted in the mobile phase, chromatographed on a C18 reversed‐phase column and analyzed by mass spectrometry via a heated nebulizer interface where they are detected by multiple reaction monitoring. The method has a chromatographic run time of less than 5 min and a linear calibration curve with a range of 1–400 ng ml−1 (r > 0.999). The between‐run precision, based on the relative standard deviation for replicate quality controls, was ≤5.5% (10 ng ml−1), 1.0% (50 ng ml−1) and 2.7% (200 ng ml−1). The between‐run accuracy was ±7.1, 3.8 and 4.8% for the above concentrations, respectively. This method was employed in a bioequivalence study of two DFZ tablet formulations (Denacen from Marjan Industria e Comercio, Brazil, as a test formulation, and Calcort from Merrell Lepetit, Brazil, as a reference formulation) in 24 healthy volunteers of both sexes who received a single 30 mg dose of each formulation. The study was conducted using an open, randomized, two‐period crossover design with a 7‐day washout interval. The 90% confidence interval (CI) of the individual geometric mean ratio for Denacen/Calcort was 89.8–109.5% for area under the curve AUC(0–24 h) and 80.7–98.5% for Cmax. Since both the 90% CI for AUC(0–24 h) and Cmax were included in the 80–125% interval proposed by the US Food and Drug Administration, Denacen was considered bioequivalent to Calcort according to both the rate and extent of absorption. Copyright © 2000 John Wiley & Sons, Ltd.

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“…Previously reported methods for determination of 21-DFZ include detection by high performance liquid chromatography 3 and liquid chromatography-mass spectrometry (LC-MS) 4,5,6 . The reported method based on LC-MS detection used the relatively tedious technique of liquid-liquid extraction (LLE) for analyte extraction from plasma 4,5,6 .…”

Section: Introductionmentioning

confidence: 99%

“…The reported method based on LC-MS detection used the relatively tedious technique of liquid-liquid extraction (LLE) for analyte extraction from plasma 4,5,6 . The other reported method used C18cartridge based solid phase extraction (SPE) extraction followed by semi-microbore liquid chromatography for determination of 21-DFZ using a high sample volume of 2ml human plasma 3 . The reported method lacks the selectivity and sensitivity offered by liquid chromatography-tandem mass spectrometry (LC-MS/MS) for high-throughput analysis of 21-DFZ.…”

Section: Introductionmentioning

confidence: 99%

A Lc-MS/MS Method for the Quantification of Deflazacort Metabolite in Human Plasma: Development, Validation and Application to a Pharmacokinetic Study

Karthikeyan¹

2013

J. Drug Delivery Ther.

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Deflazacort is a methyl-oxazoline derivative of prednisolone used for its anti-inflammatory and immunosuppressive effects. It is an inactive prodrug which is converted rapidly to its active metabolite 21-desacetyl deflazacort. A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed for the estimation of 21-desacetyl deflazacort in human plasma. Sample preparation involved simple solid phase extraction of 21-desacetyl deflazacort and internal standard. The samples were analyzed using a reversed phase column and detected using positive mode ESI tandem mass spectrometry. The LLOQ was 0.5 ng/mL and the assay was linear over the range of 0.5-100 ng/mL using a sample volume of 250µL. The method was validated for specificity, linearity, precision, accuracy and stability parameters. The method was applied to the analysis of plasma samples after oral administration of 6 mg DFZ tablets of marketed product in healthy adult subjects in a fasting bioavailability study.

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Quantitative determination of 21‐hydroxy‐deflazacort in human plasma using gradient semi‐microbore liquid chromatography

Cited by 9 publications

References 3 publications

An Investigation of the Dose Proportionality of Deflazacort Pharmacokinetics

An Investigation of the Dose Proportionality of Deflazacort Pharmacokinetics

Determination of 21-hydroxydeflazacort in human plasma by high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry. Application to bioequivalence study

A Lc-MS/MS Method for the Quantification of Deflazacort Metabolite in Human Plasma: Development, Validation and Application to a Pharmacokinetic Study

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