Determination Of Dexamethasone Research Articles

Selective Extraction and Determination of Hydrocortisone and Dexamethasone in Skincare Cosmetics: Analytical Interpretation Using Statistical Physics Formalism

Molecularly imprinted polymers (MIPs), as magnetic extraction adsorbents, are used for the selective, rapid determination and extraction of dexamethasone and hydrocortisone in skincare products. Therefore, in this paper, magnetic molecularly imprinted polymers (MMIPs) and magnetic non-molecularly imprinted polymers (MNIPs) were utilized as adsorbents to describe the adsorption phenomena of dexamethasone and hydrocortisone. This interpretation, based on a statistical physics theory, applies the multilayer model with saturation to comprehend the adsorption of the drugs. Results obtained via numerical simulation revealed that dexamethasone and hydrocortisone adsorption happens via a non-parallel orientation on the surfaces of MMIPs and MNIPs, and they also showed that the adsorption amount of the MMIPs for the template molecule was notably greater than that of the MNIPs at the same initial concentration. The adsorption energy values retrieved from the data analysis ranged between 7.65 and 15.77 kJ/mol, indicating that the extraction and determination of dexamethasone and hydrocortisone is a physisorption process. Moreover, the distribution of a site’s energy was calculated to confirm the physical nature of the interactions between adsorbate/adsorbent and the heterogeneity of the surfaces of the MMIPs and MNIPs. Finally, the thermodynamic interpretation confirmed the exothermicity and spontaneous nature of the adsorption of these drugs on the tested adsorbents.

Analytical method validation and determination of dexamethasone in divided powder using reverse phase HPLC

Dexamethasone as glucocorticoids has been widely used to reduce inflammation and tissue damage in a variety of conditions. It was commonly prescribed in combination with the other compounds such as chlorpheniramine maleate for the relief of asthma. It was important to observe the quality and safety of the combination dosage form, called pulveres or puyer in order to serve the patient oriented medication. This research aimed to develop analytical method validation and determine the content uniformity of the divided powder containing dexamethasone compounded by pharmacy in Yogyakarta and hospital in Central Java, Indonesia. A validated high performance liquid chromatography (HPLC) method was chosen to determine dexamethasone in the samples. The column of ACE 5 C18 (250 x 4.6 mm) was used in this research and the methanol:water (65:35) was used as the mobile phase at the flow rate of 1 mL/min. The UV detection was performed at 239 nm. Analytical method validation was performed on the parameters of system suitability, limit of detection, limit of quantification, accuracy, precision, and linearity. The results showed that dexamethasone contains in divided powder compounded by pharmacy in Yogyakarta and hospital in Central Java were met the acceptance requirement.

Development of an Analytical Method for the Determination of Dexamethasone in Bovine Milk Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

Development of an Analytical Method for the Determination of Dexamethasone in Bovine Milk Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

TLC-Densitometric and RP-HPLC Methods for Simultaneous Determination of Dexamethasone and Chlorpheniramine Maleate in the Presence of Methylparaben and Propylparaben.

Validated simple, sensitive, and highly selective methods are applied for the quantitative determination of dexamethasone and chlorpheniramine maleate in the presence of their reported preservatives (methylparaben and propylparaben), whether in pure forms or in pharmaceutical formulation. TLC is the first method, in which dexamethasone, chlorpheniramine maleate, methylparaben, and propylparaben are separated on silica gel TLC F254 plates using hexane-acetone-ammonia (5.5 + 4.5 + 0.5, v/v/v) as the developing phase. Separated bands are scanned at 254 nm over a concentration range of 0.1-1.7 and 0.4-2.8 μg/band, with mean ± SD recoveries of 99.12 ± 0.964 and 100.14 ± 0.962%, for dexamethasone and chlorpheniramine maleate, respectively. Reversed-phase HPLC is the second method, in which a mixture of dexamethasone and chlorpheniramine maleate, methylparaben, and propylparaben is separated on a reversed-phase silica C18 (5 μm particle size, 250 mm, 4.6 mm id) column using 0.1 M ammonium acetate buffer-acetonitrile (60 + 40, v/v, pH 3) as the mobile phase. The drugs were detected at 220 nm over a concentration range of 5-50 μg/mL, 2-90 μg/mL, 4-100 μg/mL, and 7-50 μg/mL, with mean ± SD recoveries of 100.85 ± 0.905, 99.67 ± 1.281, 100.20 ± 0.906, and 99.81 ± 0.954%, for dexamethasone, chlorpheniramine maleate, methylparaben paraben, and propylparaben, respectively. The advantages of the suggested methods over previously reported methods are the ability to detect lower concentrations of the main drugs and to show better resolution of interfering preservatives; hence, these methods could be more reliable for routine QC analyses.

Microemulsion electrokinetic chromatography with polarity switching stacking mode for the determination of dexamethasone and dexamethasone sodium phosphate: application to pharmacokinetic studies in rabbit plasma

MEEKC electropherograms of (A) a standard mixture of (2.0 μg mL−1) HCT, (1), DEX-SP, (2), and DEX, (3) and (B) the treated rabbit plasma sample.

ISOLATION, IDENTIFICATION, AND CHARACTERIZATION OF 17-OXO DEXAMETHASONE, AN OXIDATIVE DEGRADATION IMPURITY OF DEXAMETHASONE USING FLASH CHROMATOGRAPHY AND NMR/HRMS/IR

Some formulations of dexamethasone available in the market require γ-radiation sterilized dexamethasone active pharmaceutical ingredient (API). A new impurity was detected in the γ-radiation sterilized dexamethasone API and determined using gradient ultra performance liquid chromatography (UPLC) method with UV detection. This impurity was identified as the major peroxide degradation impurity of dexamethasone. This impurity standard was consequently isolated via oxidative degradation followed by flash liquid chromatography (LC) method. Using high-resolution mass spectrometry (HRMS), nuclear magnetic resonance (NMR), and infrared (IR) study the impurity was identified as 17-oxo dexamethasone (dexamethasone 17-ketone). In this method, about 600 mg of relatively pure 17-oxo dexamethasone impurity (chromatographic purity: 99.34% w/w by LC) was obtained with 1000 mg of extract loaded. This isolated 17-oxo dexamethasone impurity served as external standard for determination of percentage amounts of this impurity present in dexamethasone API and various formulation of dexamethasone. Several HPLC methods were developed and reported for the determination of dexamethasone and its related substances using UV detection. But till now there are no reports on isolation and characterization of 17-oxo dexamethasone formed during γ-radiation sterilized dexamethasone API.

Determination of Dexamethasone and Cortisol in Serum by High-Performance Giquid Chromatography with Fluorescence Detection

Determination of Dexamethasone and Cortisol in Serum by High-Performance Giquid Chromatography with Fluorescence Detection

Simultaneous Determination of Dexamethasone and Betamethasone in Swine Liver by High Performance Liquid Chromatography Tandem Mass Spectrometry with Isotope Dilution

Simultaneous Determination of Dexamethasone and Betamethasone in Swine Liver by High Performance Liquid Chromatography Tandem Mass Spectrometry with Isotope Dilution

Simultaneous Determination of Dexamethasone, Dexamethasone 21‐Acetate, and Paclitaxel in a Simulated Biological Matrix by RP‐HPLC: Assay Development and Validation

A simple and accurate reversed‐phase high performance liquid chromatography method was developed and validated for the simultaneous determination of dexamethasone, dexamethasone 21‐acetate, and paclitaxel in simulated biological matrix. Triamcinolone Acetonide was used as the internal standard (IS). A one step liquid–liquid extraction with ethyl acetate was used for sample cleanup. A gradient elution on a C−18 column with acetonitrile and 0.1% o‐phosphoric acid in water was employed to get a cleanup baseline and efficient separation of the three chemical entities. Dexamethasone and dexamethasone 21‐acetate were observed at 254 nm and paclitaxel was observed at 228 nm. The method was highly selective and the calibration curves were linear over the range of 0.25–10.0 µg/mL with a 12 min chromatographic run time. The assay method was validated in terms of accuracy, precision, absolute recovery, freeze‐thaw stability, bench top stability, and reinjection reproducibility. The lower limit of quantitation was 0.25 µg/mL for all the analytes. The intra and inter‐batch precision and accuracy were found to be well within acceptable limits (<15%). The assay is simple, reliable, and fast and is deemed suitable for application to in vitro release rate studies of these drugs from implantable devices, as well as to their in vivo pharmacokinetic studies.

Determination of Dexamethasone in Cosmetics by MEKC

A rapid and reliable method based on micellar electrokinetic capillary chromatography has been developed for the determination of dexamethasone in cosmetics. Effects of buffer composition, concentration and pH, the detection wavelength, separation voltage, and injection time were systematically investigated. The optimum conditions were: 30 mM borax buffer containing 20 mM sodium dodecyl sulfate at pH 9.0, detection at 254 nm, injection time 10 s at a height of 10 cm, and a separation voltage of 15 kV. Under these conditions, the analysis of dexamethasone in cosmetics was carried out within 6 min. The method was validated for stability, precision, linearity and accuracy. Excellent linearity was obtained in the range of 50–1,000 μg mL−1, and acceptable precision, in intra-day and inter-day analysis, was also obtained with relative standard deviation in the range of 0.19–0.86 and 2.50–4.90% for migration time and peak area ratio, respectively. The method was used to analyse eight cosmetic samples purchased locally.

HPLC Determination of Dexamethasone in Human Plasma

A sensitive high performance liquid chromatography (HPLC) method has been developed for the determination of dexamethasone in human plasma. After 1.5 mL of plasma was extracted with 4 mL of ethyl acetate containing 80 ng/mL of desoxymethasone, analysis of dexamethasone in plasma samples was carried out using a Sphereclone ODS2 column with UV detection for separation and quantification. A mixture of acetonitrile–10 mM phosphate buffer (pH 7.0) (32:68, v/v) was used as a mobile phase. The limit of quantitative (LOQ) analysis was 10 ng/mL. The accuracy of the assay was from 96.96% to 106.07%, while the intra‐ and inter‐day coefficient of variation of the same concentration range was less than 15%, except LOQ (<20%). The signals were monitored by a UV detector at 240 nm with flow‐rate of 1.0 mL/min. The method could be applied, with great success, to evaluate the bioavailability of dexamethasone in human subjects, with excellent selectivity and reproducibility and clinical study.

Micellar electrokinetic capillary chromatography as an alternative method for the determination of dexamethasone, trimethoprim, and polymyxin B.

A micellar electrokinetic capillary chromatographic method is presented which enables quantification of dexamethasone, polymyxin B and trimethoprim in synthetic mixtures and pharmaceutical products. Separation was carried out at 25 degrees C and 30 kV, with 10 mmol L(-1) borate-phosphate buffer adjusted to pH 8 as electrolyte, with 50 mmol L(-1) sodium dodecyl sulfate. Under these conditions separations were performed in 10 min. The limits of detection and quantification were approximately 2 mg L(-1) for each component, except for polymyxin B. The method was applied to different commercial formulations.

Determination of dexamethasone in feed by TLC and HPLC.

Two detection methods are described for the determination of dexamethasone in feed, which may be used as screening and confirmatory methods. The procedures were developed after studying different extraction and clean-up procedures: feed extraction was optimized using methylene chloride and hexane followed by a tandem solid-phase clean-up step with silica and C18 cartridges. The confirmatory method presented is based on normal-phase high-performance liquid chromatography on a Diol 5 microns column, with hexane-propan-2-ol (90:10 v/v) as mobile phase, followed by diode array detection and confirmation. All parameters are discussed, especially the extraction and clean-up steps. Recovery studies after application of the proposed method to different kinds of feed samples spiked with dexamethasone at levels between 120 and 1600 ng g-1 yielded a mean value of 55.4% with an overall standard deviation of 15.6%. The proposed procedure allows the determination of dexamethasone in feed at levels lower than 50 ng g-1.

Determination of dexamethasone in saliva

We conducted experiments to demonstrate that the determination of dexamethasone in saliva is a valuable tool to assess dexamethasone concentrations in the body after administration of this synthetic corticosteroid. After extraction of saliva, a RIA involving highly specific commercially available antibodies was established and evaluated. This RIA was easy to conduct, reliable, and sensitive enough to measure dexamethasone until approximately 24 h after oral administration of 1 mg per 70 kg of body weight. On the morning after the administration, the mean concentration in saliva was 540 pmol/L. Over a large range (10(3)-10(6) pmol/L), plasma concentrations correlated very well with salivary concentrations; plasma contained six times more dexamethasone than saliva.

Determination of dexamethasone in plasma of premature neonates using high-performance liquid chromatography.

A high-performance liquid chromatographic assay is described for dexamethasone in neonatal plasma. Samples (100 microliters) were extracted with ethyl acetate (1.0 ml) containing 50 ng of beclomethasone. The mobile phase of acetonitrile-0.01 M phosphate buffer (pH 7.0) (45:55, v/v) was pumped at a flow-rate of 1.0 ml/min through an Ultrasphere ODS column (5.0 microns particles). Detection was by UV absorbance at 240 nm. Calibration plots were linear (r2 > 0.999) from 10-1000 ng/ml. Within-day and between-day precision (C.V.%, coefficient of variation) between 15-900 ng/ml was 1.21-20.6%. Inaccuracy was 7.7%, or less. The minimum quantifiable concentration (C.V. approximately 20%) was 15 ng/ml. Recovery (20-1000 ng/ml) exceeded 75%. Concomitant neonatal medication did not interfere.

Determination of Dexamethasone in Plasma by High-Performance Liquid Chromatography with Chemiluminescence Detection

Determination of Dexamethasone in Plasma by High-Performance Liquid Chromatography with Chemiluminescence Detection

A selective LC/RIA for dexamethasone and its prodrug dexamethasone-21-isonicotinate in biological fluids

A combined LC/RIA procedure is described for the selective determination of dexamethasone (DEX) and its prodrug dexamethasone-21-isonicotinate (DIN) in plasma. The low affinity of the employed dexamethasone antiserum for DIN (cross-reactivity less than 0.5%) allowed the direct determination of DEX in plasma extracts. For the determination of DIN, both substances of interest were separated by LC, the DIN containing fraction was collected, hydrolysed and the generated DEX was consequently assayed by radioimmunoassay. The assay detection limits were 0.1 ng ml-1 for DEX and 0.75 ng ml-1 for DIN. For both substances, inter- and intra-day variabilities (RSDs) were 6 and 12%, respectively.

A rapid and highly sensitive method for the quantitative determination of dexamethasone in plasma, synovial fluid and tissues by combined gas chromatography/negative ion chemical ionization mass spectrometry

A new, simple and highly sensitive assay is developed for the quantitative measurement of very low levels of dexamethasone in human plasma, synovial fluid and tissues following a topical administration of the drug. Dexamethasone and the internal standard, flumethasone, are measured by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. After a three-step extraction procedure, the two compounds of interest are converted to their trimethylsilyl ether derivatives using trimethylsilylimidazole and formamide as the base catalyst. Under soft derivatization conditions only one chromatographic peak corresponding to the trisubstituted derivative is observed. The mass spectrometer is focused to monitor abundant and stable characteristic high-mass ions (m/z 446 and 464) which are generated in the ion source by an electron capture process. This assay requires only 1 ml of plasma or 0.5 ml of synovial fluid and the detection limit of the method is equal to 0.1 ng ml-1 with a relative standard deviation lower than 6%.

Liquid Chromatographic Determination and Identification Tests for Dexamethasone in Bulk Drugs and Elixirs: Collaborative Study

A normal phase liquid chromatographic method for the determination of dexamethasone in bulk drugs and elixirs was collaboratively studied by 6 laboratories. The method uses a silica column, water-modified acetic acid-methanol-methylene chloride mobile phase, cortisone internal standard, and photometric detection at 254 nm. Collaborators were supplied blind duplicate samples of 3 bulk drugs, 2 commercial elixirs, and 1 authentic elixir. Dexamethasone elixir dosage level is 0.5 mg/5 mL. Mean recovery of dexamethasone from the authentic elixir formulated to contain 0.471 mg/5 mL was 94.5%. (Authentic elixirs were found to stabilize about 6% below the theoretical concentration.) Mean recovery for the bulk drugs was between 97.1 and 100.1%. Mean coefficients of variation for bulk drug and elixir samples were less than 0.8% and 3.6%, respectively. Identification tests for dexamethasone by thin-layer chromatography, infrared spectroscopy, and relative LC retention times, as well as the gas chromatographic determination of alcohol in the elixirs were also collaboratively studied. Mean recovery of alcohol from the synthetic elixir was 98.6%. The mean coefficient of variation for alcohol for all samples analyzed was less than 1.4%. The LC method for dexamethasone in drug substance and elixirs, the identification tests, and the GC method for alcohol in dexamethasone elixirs have been adopted official first action.

Determination of dexamethasone (DXM) levels in plasma by HPLC and RIA

Determination of dexamethasone (DXM) levels in plasma by HPLC and RIA