An easy, eclectic, precise high-Performance Liquid Chromatographic (HPLC) procedure was evolved and validated to estimate of Piroxicam and Codeine phosphate. Chromatographic demarcation was accomplished on a C18 column [Use BDS Hypersil C18, 5μ, 150 x 4.6 mm] using a mobile phase of methanol: phosphate buffer (60:40, v/v, pH=2.3), the flow rate was 1.1 mL/min, UV detection was at 214 nm. System Suitability tests (SSTs) are typically performed to assess the suitability and effectiveness of the entire chromatography system. The retention time for Piroxicam was found to be 3.95 minutes and 1.46 minutes for Codeine phosphate. The evolved method has been validated through precision, limit of quantitation, specificity, limit of detection linearity and accuracy. (LOD) was 1.92 mg/mL and (LOQ) was 6.336 mg/mL for Piroxicam, whereas (LOD) for Codeine phosphate was 0.29 mg/mL and (LOQ) was 0.95 mg/mL. Piroxicam and Codeine phosphate showed a linear signal in the domain of 5-50 µg/mL for each compound. This research presided to evolve and validate an HPLC method, and the proposed procedure can be used to estimate these drugs in their combined dosage forms.
A chemometric method, partial least squares regression (PLS) was applied for the simultaneous determination of piroxicam (PIR), naproxen (NAP), diclofenac sodium (DIC), and mefenamic acid (MEF) in synthetic mixtures and commercial formulations. The proposed method is based on the use of spectrophotometric data coupled with PLS multivariate calibration. The Spectra of drugs were recorded at concentrations in the linear range of 1.0 - 10 μg mL-1 for NAP and from 1.0 - 20 μg mL-1 for PIR, DIC, and MEF. 34 sets of mixtures were used for calibration and 10 sets of mixtures were used for validation in the wavelength range of 200 to 400 nm with the wavelength interval λ = 1 nm in methanol. This method has been used successfully to quant
... Show MoreA simple reverse-phase high performance liquid chromatographic method for the simultaneous analysis (separation and quantification) of furosemide (FURO), carbamazepine (CARB), diazepam (DIAZ) and carvedilol (CARV) has been developed and validated. The method was carried out on a NUCLEODUR® 100-5 C18ec column (250 x 4.6 mm, i. d.5μm), with a mobile phase comprising of acetonitrile: deionized water (50: 50 v/v, pH adjusted to 3.6 ±0.05 with acetic acid) at a flow rate 1.5 mL.min-1 and the quantification was achieved at 226 nm. The retention times of FURO, CARB, DIAZ and CARV were found to be 1.90 min, 2.79 min, 5.39 min and 9.56 min respectively. The method was validated in terms of linearity, accuracy, precision, limit of detection and li
... Show MoreChromatographic and spectrophotometric methods for the estimation of mebendazole in
pharmaceutical products were developed. The flow injection method was based on the oxidation of
mebendazole by a known excess of sodium hypochlorite at pH=9.5. The excess sodium hypochlorite is then
reacted with chloranilic acid (CAA) to bleach out its color. The absorbance of the excess CAA was recorded
at 530 nm. The method is fast, simple, selective, and sensitive. The chromatographic method was carried out
on a Varian C18 column. The mobile phase was a mixture of acetonitrile (ACN), methanol (MeOH), water
and triethylamine (TEA), (56% ACN, 20% MeOH, 23.5% H2O, 0.5% TEA, v/v), adjusted to pH = 3.0 with
1.0 M hy
The novel Vierordt’s approach, or simultaneous equation method, was created and validated for the concurrent determination of vincristine sulfate (VCS) and bovine serum albumin (BSA) in pure solutions utilizing UV spectrophotometry. It is simple, precise, economical, rapid, reliable, and accurate. This method depends on measuring absorbance at two wavelengths, 296 nm and 278 nm, which correspond to the λmax of VCS and BSA in deionized water, respectively. The calibration curves of VCS and BSA are linear at concentration ranges of 10–60 μg/mL and 200–1600 μg/mL, with correlation coefficient values (R2) of 1 and 0.999, respectively. The limits of detection (LOD) and quantification (LO
... Show MoreTwo simple methods spectrophotometric were suggested for the determination of Cefixime (CFX) in pure form and pharmaceutical preparation. The first method is based without cloud point (CPE) on diazotization of the Cefixime drug by sodium nitrite at 5Cº followed by coupling with ortho nitro phenol in basic medium to form orange colour. The product was stabilized and measured 400 nm. Beer’s law was obeyed in the concentration range of (10-160) μg∙mL-1 Sandell’s sensitivity was 0.0888μg∙cm-1, the detection limit was 0.07896μg∙mL-1, and the limit of Quantitation was 0.085389μg∙mL-1.The second method was cloud point extraction (CPE) with using Trtion X-114 as surfactant. Beer
... Show MoreIn the present work, a kinetic study was performed to the extraction of phosphate from Iraqi Akashat phosphate ore using organic acid. Leaching was studied using lactic acid for the separation of calcareous materials (mainly calcite). Reaction conditions were 2% by weight acid concentration and 5ml/gm of acid volume to ore weight ratio. Reaction time was taken in the range 2 to 30 minutes (step 2 minutes) to determine the reaction rate constant k based on the change in calcite concentration. To determine value of activation energy when reaction temperature is varied from 25 to 65 , another investigation was accomplished. Through the kinetic data, it was found that selective leaching was controlled by
... Show MoreThe aim of this work was to develop and validate a rapid and low cost method for estimation of ibuprofen in pharmaceutical suspensions using Reverse-Phase High Performance Liquid Chromatography. The proposed method was conducted and validated according to International Conference on Harmonization (ICH) requirements. The chromatographic parameters were as follows: column of octyldecylsilyl C18 with dimensions (150 × 4.6) mm, mobile phase composed of acetonitrile with phosphoric acid with a ratio of 50 to 50 each using isocratic mode, flow rate of 1.5 mL/min and injection volume of 5 μL. The detection was carried out using UV detector at 220 nm. The method was validated and showed short retention time for ibuprofen peak at 7.651 min, wit
... Show MoreIn this work, a simple and very sensitive cloud point extraction (CPE) process was developed for the determination of trace amount of metoclopramide hydrochloride (MTH) in pharmaceutical dosage forms. The method is based on the extraction of the azo-dye results from the coupling reaction of diazotized MTH with p-coumaric acid (p-CA) using nonionic surfactant (Triton X114). The extracted azo-dye in the surfactant rich phase was dissolved in ethanol and detected spectrophotometrically at λmax 480 nm. The reaction was studied using both batch and CPE methods (with and without extraction) and a simple comparison between the two methods was performed. The conditions that may be affected by the extraction process and the sensitivity of m
... Show MoreA new, accurate, precise and economic two spectrophotometric methods for determination of Paracetamol (Par), Ibuprofen (Ibu), and Caffeine (Caf) were suggested. Those methods were the first and second ratio derivative spectrum using a double devisor. Par, Ibu, and Caf showed many useful peaks for their quantified determination. The validity of all analysis modes for determination of the three compounds, peak to baseline, peak area and peak to peak were according to ICH. The linearity of two methods was between 5 µg/ml as a lower concentration and 50 µg/ml as the highest concentration for three compounds. Recovery percentage was around 100% and relative standard deviation was less than 2.6%. The methods were applied successfully in the
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