Simultaneous determination of paracetamol,phenylephrine hydrochloride and chlorpheniramine maleate in pharmaceutical preparations using multivariate calibration 1

Resolution of binary mixtures of paracetamol, phenylephrine hydrochloride and chlorpheniramine maleate with minimum sample pre-treatment and without analyte separation has been successfully achieved by methods of partial least squares algorithm with one dependent variable, principal component regression and hybrid linear analysis. Data of analysis were obtained from UV–vis spectra of the above compounds. The method of central composite design was used in the ranges of 1–15 mg L^?1 for both calibration and validation sets. The models refinement procedure and their validation were performed by cross-validation. Figures of merit such as selectivity, sensitivity, analytical sensitivity and limit of detection were determined for all three compounds. The procedure was successfully applied to simultaneous determination of the above compounds in pharmaceutical tablets.     

Simultaneous quantification of nimesulide,phenylpropanolamine, caffeine and chlorpheniramine in rat plasma by RP–HPLC/PDA method and application to pharmacokinetic studies in healthy rat subjects

Simultaneous determination of nimesulide, phenylpropanolamine, chlorpheniramine and caffeine in rat plasma by reversed-phase high performance liquid-chromatography (RP–HPLC) with photodiode array (PDA) detection method was developed and validated. Sample preparation based on a simple extraction procedure consisting of deproteination and extraction with methanol solution followed by volume make up with the aqueous component of the mobile phase obtained best recoveries of the analytes. The chromatographic conditions were optimized and the analytes were separated on XBridge™ C₁₈ (3.5 μm, 4.6 × 150 mm) column in isocratic elution with the mobile phase composition of acetonitrile and 10 mM ammonium acetate buffer (pH 4.0, 0.1% formic acid) (18:82 v/v%) at the flow rate of 1 mL min⁻¹ and the effluents were monitored in the wavelength range of 220–275 nm. The method was linear for all analytes over the following concentration (ng mL⁻¹) ranges: nimesulide 250–4000; phenylpropanolamine 100–1500; chlorpheniramine 20–500; and caffeine 10–100. Acceptable precision, accuracy and recoveries were obtained for quality control (QC) samples at three concentrations (low QC, middle QC and high QC). The percentage of relative standard deviation (% RSD) of Inter and intra-run precision of all molecules was <15% and the percentage of accuracy was 100 ± 10. The analytes were more stable in rat plasma at different storage conditions. Finally the method was efficiently applied to pharmacokinetics study in rat plasma.     

Determination of phenylephrine hydrochloride and chlorpheniramine maleate in binary mixture using chemometric-assisted spectrophotometric and high-performance liquid chromatographic-UV methods

Four methods have been developed for the simultaneous determination of phenylephrine hydrochloride and chlorpheniramine maleate without previous separation. In the first method both drugs are determined using first derivative UV spectrophotometry, with zero-crossing measurement. The second method depends on first derivative of the ratios spectra. The third method describes the use of multivariate spectrophotometric calibration for the simultaneous determination of the analyzed binary mixture where the resolution is accomplished by using partial least squares (PLS) regression analysis. In the fourth method (HPLC), a reversed-phase column and a mobile phase of methanol:water:acetonitrile (80:12:8 v/v/v/) at 0.9 ml/min flow rate have been used to separate both drugs with a UV detection at 270 nm. All the proposed methods are extensively validated. They have the advantage to be economic and time saving. All the described methods can be readily utilized for analysis of pharmaceutical formulations. The results obtained using the proposed methods are statistically analyzed and compared with some reported methods.     

Stability indicating method for the determination of paracetamol in its pharmaceutical preparations by TLC densitometric method

Simple, sensitive and accurate thin layer procedure was described for a quantitative determination of paracetamol in its bulk powder and in its pharmaceutical dosage forms in the presence of its degradation product. The method consists of dissolving the drug in methanol and then spotting the solution on a thin layer of silica gel G254. Paracetamol was separated on silica gel using the mixture of the mobile phase, ethyl acetate: benzene: acetic acid in a ratio (1:1:0.05 v/v/v).Absorbance measurements (detection of reflectance) of the separated drug were carried out at 250 nm. Calibration curves were established in the concentration range of 5–20 mcg/spot for paracetamol. Quantitation is achieved by comparing the area under the peaks obtained from scanning the thin layer chromatographic plates in a spectrodensitometer. The method has been successfully applied to pharmaceutical preparations (capsules) and the results obtained were statistically compared with those obtained by applying the reference method.     

Simultaneous HPLC-UV Determination of Lactic Acid,Glycolic Acid,Glycolide, Lactide and Ethyl Acetate in Monomers for Producing Biodegradable Polymers

A simple, rapid high-performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of glycolic acid, lactic acid, glicolide, lactide and ethyacetate in monomers for obtaining biopolymers. The separation was effected on the reversed-phase C18 column 250mm×4.6 mm with particle size 5 μ using a mobile phase mixture buffer and acetonitrile in a ratio 88:12 v/v and elution was isocratic at a flow-rate of 1.0 mL/min. The determinations were performed with a UV-Vis detector at 200 nm. The volume of the injected sample was 20 μL. Detection limits for acids and its dimers (glycolic acid, lactic acid, glicolide, lactide) and ethylacetate range between 82 and 182 ng/mL. The analytes are separated in 13 min. Recovery studies showed good results for all solutes (99–102%). The method is linear for all compounds over the concentration range tested, and shows good precision and accuracy, making it suitable for quantitation of acids and its dimers (glycolic acid, lactic acid, glicolide, lactide) and ethyl acetate in monomers.     

Development of a stability-indicating high performance liquid chromatography method for assay of erythromycin ethylsuccinate in powder for oral suspension dosage form

In this study an effective method was developed to assay erythromycin ethylsuccinate for an oral suspension dosage form. The chromatographic separation was achieved on an X-Terra™ C₁₈ analytical column. A mixture of acetonitrile–ammonium dihydrogen phosphate buffer (0.025 mol L^-1) (60:40, V/V) (pH 7.0) was used as the mobile phase, effluent flow rate monitored at 1.0 mL min⁻¹, and UV detection at 205 nm. In forced degradation studies, the effects of acid, base, oxidation, UV light and temperature were investigated showing no interference in the peak of drug. The proposed method was validated in terms of specificity, linearity, robustness, precision and accuracy. The method was linear at concentrations ranging from 400 to 600 μg mL⁻¹, precise (intra- and inter-day relative standard deviations <0.65), accurate (mean recovery; 99.5%). The impurities and degradation products of erythromycin ethylsuccinate were selectively determined with good resolution in both the raw material and the final suspension forms. The method could be useful for both routine analytical and quality control assays of erythromycin ethylsuccinate in commercial powder for an oral suspension dosage form and it could be a very powerful tool to investigate the chemical stability of erythromycin ethylsuccinate.     

The standard molar enthalpy of formation,molar heat capacities,and thermal stability of anhydrous caffeine

The constant-volume energy of combustion of crystalline anhydrous caffeine (C₈H₁₀N₄O₂) in α (lower temperature steady) crystal form was measured by a bomb combustion calorimeter, the standard molar enthalpy of combustion of caffeine at T = 298.15 K was determined to be −(4255.08 ± 4.30) kJ · mol⁻¹, and the standard molar enthalpy of formation was derived as −(322.15 ± 4.80) kJ · mol⁻¹. The heat capacity of caffeine in the same crystal form was measured in the temperature range from (80 to 387) K by an adiabatic calorimeter. No phase transition or thermal anomaly was observed in the above temperature range. The thermal behavior of the compound was further examined by thermogravimetry (TG), differential thermal analysis (DTA) over the range from (300 to 700) K and by differential scanning calorimetry (DSC) over the range from (300 to 540) K, respectively. From the above thermal analysis a (solid–solid) and a (solid–liquid) phase transition of the compound were found at T = (413.39 and 509.00) K, respectively; and the corresponding molar enthalpies of these transitions were determined to be (3.43 ± 0.02) kJ · mol⁻¹for the (solid–solid) transition, and (19.86 ± 0.03) kJ · mol⁻¹ for the (solid–liquid) transition, respectively.     

Ion-pairing and reversed phase liquid chromatography for the determination of three different quinolones: Enrofloxacin,lomefloxacin and ofloxacin

Two simple and sensitive high performance liquid chromatographic (HPLC) methods have been developed for the simultaneous determination of three different quinolones: enrofloxacin, lomefloxacin and ofloxacin in their pure and dosage forms, one with reversed phase HPLC and the other with ion-pair HPLC. In reversed phase HPLC, method (A), the mobile phase consists of 2.18% aqueous solution of KH₂PO₄ with pH adjusted to 2.4 ± 0.2 with acetonitrile (80:20; v/v), the mobile phase pumped at flow rate of 1.2 ml min^?1. A Neucleosil C₁₈ column (10 μm, 100 Å), 250 mm length × 4.6 mm diameter was utilized as stationary phase. Detection was affected spectrophotometrically at 294 nm. While in ion-pair HPLC, method (B), the mobile phase was aqueous solution of 0.65% sodium perchlorate and 0.31% ammonium acetate adjusted to pH 2.2 ± 0.2 with orthophosphoric acid: acetonitrile (81:19; v/v), the mobile phase pumped at flow rate of 1.5 ml min^?1. A μ bondapack C₁₈ column (10 μm, 100 Å), 250 mm length × 4.6 mm diameter was utilized as stationary phase. Detection was affected spectrophotometrically at 294 nm. Linearity ranges for enrofloxacin, lomefloxacin and ofloxacin were 4.0–108, 7.0–112 and 8.0–113 μg ml^?1, respectively using method A and 8.0–112, 7.0–112 and 5.0–105 μg ml^?1, respectively applying method B. Minimum detection limits obtained were 0.013, 0.023 and 0.035 μg ml^?1 for enrofloxacin, lomefloxacin and ofloxacin, respectively using method A, and 0.028, 0.023 and 0.011 μg ml^?1 using method B. The proposed methods were further applied to the analysis of enrofloxacin in injection and tablets containing the ofloxacin and lomefloxacin drugs, and the results were satisfied.     

High-performance thin layer chromatography method for estimation of andrographolide in herbal extract and polyherbal formulations

A new, simple, sensitive, precise and robust high-performance thin layer chromatographic (HPTLC) method was developed for the estimation of andrographolide in herbal extracts and pharmaceutical dosage forms. Analysis of andrographolide was performed on TLC aluminium plates pre-coated with silica gel 60F-254 as stationary phase. Linear ascending development was carried out in twin trough glass chamber saturated with chloroform:toluene:methanol (66:26:8, v/v/v) at room temperature (25 ± 2 °C). The R_f value of andrographolide was found to be 0.49. Camag TLC scanner III was used for spectrodensitometric scanning and analysis in absorbance mode at 229 nm. The system was found to give compact spots for andrographolide (R_f value of 0.49). The data for calibration plots showed good linear relationship with r² = 0.9986 in the concentration range of 200 ng to 1000 ng with respect to peak area. The present method was validated by precision, recovery, robustness and reproducibility according to ICH guidelines. The limits of detection and quantification were determined and it was found to be 3.5 and 11.7 ng, respectively. Statistical analysis of the data showed that the method is reproducible and selective for estimation of andrographolide.     

Photochemical vapor generation of carbonyl for ultrasensitive atomic fluorescence spectrometric determination of cobalt

UV photochemical vapor generation (photo-CVG) as sample introduction was first adapted for determination of ultratrace cobalt by atomic fluorescence spectrometry (AFS). Cobalt volatile species can be generated when the buffer system of formic acid and formate containing Co (II) is exposed to UV radiation. The generated gaseous products were separated from liquid phase within a gas–liquid separator and then transported to AFS for determination of cobalt. Factors affecting the efficiency of photo-CVG were investigated in detail, including type and concentration of low molecular weight (LMW) organic acid, buffer system, UV irradiation time, reaction temperature, carrier gas flow rate and hydrogen flow rate. With 4% (v/v) HCOOH and 0.4 mol L^− 1 HCOONa buffer solution, 150 s irradiation time and 15 W low pressure mercury lamp, a generation efficiency of 23–25% was achieved. A limit of detection (LOD) of 0.08 ng mL^− 1 without any pre-concentration procedure and a precision of 2.2% (RSD, n = 11) at 20 ng mL^− 1 were obtained under the optimized conditions. The proposed method was successfully applied in the analysis of several simple matrix real water samples.     

HPLC-PDA analysis of ACE-inhibitors,hydrochlorothiazide and indapamide utilizing design of experiments

A simple, rapid, precise, accurate and sensitive high performance liquid chromatographic method has been developed for simultaneous determination of ACE inhibitors with hydrochlorothiazide and indapamide in pharmaceutical formulations. ‘Design of Experiments’ (DoE) using ‘central composite design’ (CCD) was applied to facilitate method development and optimization. Mobile phase was optimized utilizing response surface methodology using Design Expert software. Chromatographic separation was achieved on Hypersil®-Gold C₁₈ (100 × 4.6 mm, 3 μm, Thermo Fisher Scientific, USA), column at 25 °C. The mobile phase was 58% buffer (5 mM KH₂PO₄, containing triethylamine 0.25 ml/L), 25% acetonitrile and 17% methanol (pH adjusted to 2.8 ± 0.1). The analysis was performed at 215 nm. The mobile phase flow rate was 1.0 ml/min and injection volume 10 μl. The method was validated for linearity, limits of quantitation and detection, accuracy, precision, ruggedness and robustness as per the International Conference on Harmonization (ICH) guidelines. Calibration curves (for lisinopril, hydrochlorothiazide, captopril, imidapril, perindopril, indapamide and trandolapril) were linear in the concentration range of 5–35 μg/ml. The limit of detection and limit of quantitation for experimental drugs ranged from 0.03 to 0.61 and 0.08–1.84 μg/ml respectively.     

Development of efficient SPE–TLC method and evaluation of biological interactions of contraceptives with progesterone receptors

TLC–SPE methodologies were developed to ascertain biological interactions of norethindrone acetate and dydrogesterone contraceptives with plasma progesterone receptor proteins. TLC solvent system for plain and Cu(II) impregnated silica gel plates was n-hexane-n-butanol (90:10, v/v), which took 20 min to run up to 10.0 cm. The best separation was on Cu(II) impregnated plates due to maximum difference in R_f values and compact spots. The optimized SPE conditions were pH 2.0 and 3.0 of phosphate buffer (50 mM) for norethindrone acetate and dydrogesterone, respectively. The flow rate of plasma and eluting solvent (methanol) through C₁₈ cartridge was 0.10 mL/min. The interactions of these contraceptives with progesterone receptor proteins were analysed by TLC–SPE results, which were supported by modelling using PyMOL and Autodoc4 softwares. The dydrogesterone was found to be bound strongly than norethindrone acetate. Attempts have been made to discuss the drugs’ interactions at chemo-supramolecular level.     

Preparation and characterization of nanocomposite,silica aerogel,activated carbon and its adsorption properties for Cd (II) ions from aqueous solution

A novel composite adsorbent, silica aerogel activated carbon was synthesized by sol-gel process at ambient pressure drying method. The composite was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and Nitrogen adsorption/desorption isotherms (BET).In the present study, the mentioned adsorbent was used moderately for the removal of cadmium ions from aqueous solutions and was compared with two other adsorbents of cadmium, activated carbon and silica aerogel. The experiments of Cd adsorption by adsorbents were performed at different initial ion concentrations, pH of the solution, adsorption temperature, adsorbent dosage and contact time. Moreover, the optimum pH for the adsorption was found to be 6.0 with the corresponding adsorbent dosage level of 0.1 g at 60 °C temperature. Subsequently, the equilibrium was achieved for Cd with 120 min of contact time.Consequently, the results show that using this composite adsorbent could remove more than 60% of Cd under optimum experimental conditions. Langmuir and Freundlich isotherm model was applied to analyze the data, in which the adsorption equilibrium data were correlated well with the Freundlich isotherm model and the equilibrium adsorption capacity (q_e) was found to be 0.384 mg/g in the 3 mg/L solution of cadmium.     

Solvation consequences of polymer PVP with biological buffers MES,MOPS, and MOPSO in aqueous solutions

Densities and viscosities were measured for the aqueous buffer (MES, MOPS, or MOPSO) solutions containing different concentrations of polyvinylpyrrolidone (PVP) (5, 10, 15, 20 and 30) mass% at temperatures from (298.15 to 318.15) K under atmospheric pressure. The DFT calculations were also performed and the binding energies of the possible (PVP + buffer) complexes were obtained. The experimental and computational results reveal the interactions of the PVP with the constituent compounds in the aqueous buffer solutions. Additionally we have explored the solvation behavior of the buffers by measuring the densities and the viscosities data of the aqueous buffer solutions from (0.0 to 1.0) mol · kg⁻¹ at temperatures from (298.15 to 318.15) K. The viscosity results were correlated with the Jones–Dole equation. The correlated results confirmed that all the investigated buffers behave as Kosmotropes (structure makers).     

New,simple and validated kinetics spectrophotometric method for determination of moxifloxacine in its pharmaceutical formulations

The objective of this research was to develop a kinetic spectrophotometric method for determination of moxifloxacine (MOXF) in pure form and pharmaceutical formulations. The method was based on the formation of a colored N-vinyl chlorobenzoquinone derivative of MOXF by its reaction with 2,3,5,6-tetrachloro-1,4-benzoquinone in presence of acetaldehyde.The formation of the colored product was monitored spectrophotometrically by measuring the absorbance at 652 nm. Factors affecting the reaction were studied and optimized. The stoichiometry of the reaction was determined, and the reaction pathway was postulated. The activation energy of the reaction was calculated and found to be 6.65 kJ mol^?1. Under the optimized conditions, the initial rate and fixed time (at 5 min) methods were utilized for constructing the calibration graphs. The graphs were linear in concentration ranges 5–100 and 15–150 μg ml^?1 with limit of detection of 2.0 and 5.0 μg ml^?1 for the initial rate and fixed time methods, respectively. The analytical performance for both methods was fully validated, and the results were satisfactory. No interference was observed from the excipients that are commonly present in the pharmaceutical formulations. The proposed method was successfully applied to the determination of MOXF in its pharmaceutical formulations. The label claim percentages were 101.25 ± 0.73% and 100.92 ± 0.65% for the initial rate and fixed time method, respectively. Statistical comparison of the results with those obtained by a reference spectrophotometric method showed excellent agreement between the accuracy and precision of the two methods. The proposed method has great value in its application to the analysis of MOXF in quality control laboratories.     

Development and validation of a UPLC method for quantification of antiviral agent,Acyclovir in lipid-based formulations

PurposeThe objective of the current study is to evaluate the Ultra Performance Liquid Chromatography (UPLC) method for quantification of Acyclovir in lipid-based formulations.MethodA simple, rapid, reliable and precise reversed phase UPLC method has been developed and validated according to the regulatory guidelines, which composed of isocratic mobile phase; 0.25% formic acid (FA) in Milli-Q water with a flow rate of 0.5 ml/min, and column BEH C18 (2.1 × 50 mm, 1.7 μm). The detection was carried out at 254 nm.ResultsThe developed UPLC method was found to be rapid (1.2 min run time), selective with well resoluted Acyclovir peak (0.89 min) from different lipid matrices and sensitive (Limit of Detection (LOD) was 0.3 ppm and Lower Limit of Quantification (LLOQ) was 1 ppm). The accuracy and precision were determined and were perfectly matching with the standard FDA limits.ConclusionThe study showed that the proposed UPLC method can be used for the assessment of drug purity, stability, solubility and lipid-formulation release profile with no interference of excipients or related substances of active pharmaceutical ingredient.     

Electrochemical detection of perchloroethylene using differential pulse voltammetry

We demonstrate the application of differential pulse voltammetry (DPV) for the electrochemical detection of perchloroethylene (PCE) on an unmodified glassy carbon electrode surface. Detection sensitivity was substantially improved using DPV, in which dechlorination was denoted by a cathodic peak observed at approximately − 0.6 V (vs Ag/AgCl). Peak current intensity was found to correlate linearly with concentration over a tested range of 0 to 10 μM. The utility of this technique was subsequently evaluated for PCE-spiked environmental samples containing either Methylobacterium adhaesivum (1 × 10⁶ cells/mL) or creek water (10% v/v). In all environmental samples, a linear dynamic range was also observed from approximately 0 to 10 μM. The limit of detection was determined to be 0.3 μM in blank buffer, 0.4 μM in bacteria-containing samples and 1.2 μM in creek water samples.     

Stability-indicating liquid chromatography for determination of clopidogrel bisulfate in tablets: Application to content uniformity testing

The present study describes a simple stability-indicating reversed-phase HPLC assay for antiplatelet drug, clopidogrel bisulfate. Separation of the drug and the degradation products, under stress conditions was successfully achieved on a C-18 column utilizing 0.01 M Na₂HPO₄ (pH 4): acetonitrile in the ratio 80:20 v/v, pumped at a flow rate of 0.5 ml min^?1 with UV detection at 235 nm. The retention time of clopidogrel was 6.84 min. The method was satisfactorily validated with respect to linearity, precision, accuracy, selectivity, sensitivity and ruggedness. The response was linear in the range of 0.2–3.5 μg ml^?1 with detection limit 0.079 μg ml^?1. The suggested method was successfully applied for the analysis of clopidogrel in bulk and in commercial tablets. The results were favorably compared to those obtained by a reference method. The proposed method was successfully applied to the content uniformity testing of tablets and for determination of clopidogrel in presence of its co-administered drug, acetyl salicylic acid.     

Trace Cd,Co, and Pb elements distribution during Sulcis coal pyrolysis: GFAAS determination with slurry sampling technique

A simple and fast method based on graphite furnace atomic absorption spectrometry (GF AAS) and slurry sampling technique (SlS) was developed to determine trace Cd, Co and Pb in high-sulphur coal (Sulcis, Italy) and coal chars derived at 600, 750 and 950 °C under N₂ atmosphere for developing a clean coal for electricity production. The proposed method was then coupled to a four-step sequential chemical extraction method for assessment of metals distribution in coaled samples. The slurries were prepared by varying sample mass (1–50 mg), volume (1–3 mL) and kind of dispersing medium (1% v/v Triton X-100 and 2 N HNO₃), and sonication time (5–30 min). Pyrolysis/atomization temperatures as well carrier gas flow rate were optimised. Pd(NO₃)₂ and NH₄H₂PO₄ were employed to stabilize Cd and Pb, respectively, in the pyrolysis stage of furnace program. The use of HNO₃ as dispersing agent was found to be effective in lowering the high level of background absorption on the Cd analytical signal produced by raw coal matrix. Conversely, coal charred samples did not show significantly level of background interferences, so that Triton X-100 dispersing agent could be used for all analytes. Calibration curve against acid-matched standards was allowed for Cd, whereas the standard addition calibration was used for Co and Pb owing to chemical matrix interferences. The precision, expressed as relative standard deviation (% RSD, n = 5), was better than 5% for Cd, Co, and Pb at 1, 10, and 15 μg L^? 1 levels, respectively. The accuracy of the analytical method was checked by analyzing a BCR No. 182 steam coal certificated reference material and the results were in good agreement with certificated and informed values. The solid detection limits (3σ_blank) were as low as 0.001 Cd, 0.01 Co, and 0.01 Pb mg kg^? 1, using 30 mg sample mass and slurry concentration of 30 m v^? 1 for Cd, and 50 mg sample mass and 50 m v^? 1 slurry concentration for Co and Pb. The content of elements in Sulcis coal was found to be 0.33 Cd, 4.0 Co, and 3.8 Pb mg kg^? 1 and mostly associated to sulphates and di-sulphides as indicated by the leaching test. Under pyrolysis conditions Cd significantly volatilised (about 64%) at temperature higher than 600 °C, whereas residue chars at 950 °C are enriched in Co and Pb up to 20%. The proposed method is suitable for routine metals monitoring in coaled samples.     

Synthesis,characterization and batch assessment of groundwater fluoride removal capacity of trimetal Mg/Ce/Mn oxide-modified diatomaceous earth

In this study, trimetal Mg/Ce/Mn oxide-modified diatomaceous earth (DE) was synthesized at optimal conditions. Comparison of the SEM images and the results of EDX analyses of the raw and the modified DE confirmed the surface modification of the raw DE with the trimetal oxide. Groundwater fluoride removal capacity of the sorbent was evaluated by batch method at various defluoridation conditions. At a sorbent dosage of 0.6 g/100 mL (contact time: 60 min, mixing speed of 200 rpm and temperature: 297 K), the fluoride removal was >93% for solutions containing initial fluoride concentration of 10–60 mg/L. Sorbent’s optimum fluoride uptake capacity was 12.63 mg/g at the initial fluoride concentration of 100 mg/L. Fluoride removal was >91% for solutions with initial pH range of ∼4–11 (initial fluoride concentration: 9 mg/L, sorbent dosage: 0.6 g/100 mL). Appraisal of the effect of co-existing anions on fluoride removal showed that CO₃²⁻ would reduce the amount of fluoride removed from solution, while other anions such as PO₄³⁻, NO₃⁻ and SO₄²⁻ had no observable effect. K₂SO₄ solution was found to be most suitable for regeneration of spent Mg/Ce/Mn oxide-modified DE compared to Na₂CO₃ and NaOH. The mechanism of fluoride removal at pH > 5.45 (pHpzc = 5.45) occurred by exchange of hydroxyl groups on surface of sorbent with fluoride ions from solution. Sorption data fitted better to Langmuir isotherm and pseudo-second-order model. External diffusion was observed to be the sorption rate limiting factor.