Development of alternative methods for the determination of raloxifene hydrochloride in tablet dosage form

Three methods are proposed for the quantitative determination of raloxifene hydrochloride in pharmaceutical dosage form: ultraviolet method (UV) high performance liquid chromatography (HPLC) and micellar capillary electrophoresis (MEKC). These methods were developed and validated and showed good linearity, precision and accuracy. Also they demonstrated to be specific and robust. The HPLC and MEKC methods were tested in regards to be stability indicating methods and they showed to have this attribute. The UV method used methanol as solvent and optimal wavelength at 284 nm, obeying Lambert-Beer law in these conditions. The chromatographic conditions for the HPLC method included: NST column C18 (250 x 4.6 mm x 5 µm), mobile phase water:acetonitrile:triethylamine (67:33:0,3 v/v), pH 3.5, flow rate 1.0 mL min-1, injection volume 20.0 µl, UV detection 287 nm and analysis temperature 30 °C. The MEKC method was performed on a fused-silica capillary (40 cm effective length x 50 µm i.d.) using as background electrolyte 35.0 mmol L-1 borate buffer and 50.0 mmol L-1 anionic detergent sodium dodecyl sulfate (SDS) at pH 8.8. The capillary temperature was 32°C, applied voltage 25 kV, UV detection at 280 nm and injection was perfomed at 45 mBar for 4 s, hydrodimanic mode. In this MEKC method, potassium diclofenac (200.0 µg mL-1) was used as internal standard. All these methods were statistically analyzed and demonstrated to be equivalent for quantitative analysis of RLX in tablets and were successfully applied for the determination of the drug.

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Eco-Friendly Green Liquid Chromatographic Separations of a Novel Combination of Azelastine and Fluticasone in the Presence of their Pharmaceutical Dosage form Additives

Current Analytical Chemistry ◽

10.2174/1573411014666180727130722 ◽

2020 ◽

Vol 16 (3) ◽

pp. 277-286

Author(s):

Amal A. El-Masry ◽

Mohammed E. A. Hammouda ◽

Dalia R. El-Wasseef ◽

Saadia M. El-Ashry

Keyword(s):

Lower Limit ◽

Dosage Form ◽

Limit Of Detection ◽

Sodium Dodecyl ◽

Uv Detection ◽

Simultaneous Estimation ◽

Limit Of Quantification ◽

Chromatographic Separations ◽

Pharmaceutical Dosage Form ◽

Liquid Chromatographic

Background: The first highly sensitive, rapid and specific green microemulsion liquid chromatographic (MELC) method was established for the simultaneous estimation of fluticasone propionate (FLU) and azelastine HCl (AZL) in the presence of their pharmaceutical dosage form additives (phenylethyl alcohol (PEA) and benzalkonium chloride (BNZ)). Methods: The separation was performed on a C18 column using (o/w) microemulsion as a mobile phase which contains 0.2 M sodium dodecyl sulphate (SDS) as surfactant, 10% butanol as cosurfactant, 1% n-octanol as internal phase and 0.3% triethylamine (TEA) adjusted at pH 6 by 0.02 M phosphoric acid; with UV detection at 220 nm and programmed with flow rate of 1 mL/min. Results: The validation characteristics e.g. linearity, lower limit of quantification (LOQ), lower limit of detection (LOD), accuracy, precision, robustness and specificity were investigated. The proposed method showed linearity over the concentration range of (0.5-25 µg/mL) and (0.1-25 µg/mL) for FLU and AZL, respectively. Besides that, the method was adopted in a short chromatographic run with satisfactory resolution factors of (2.39, 3.78 and 6.74 between PEA/FLU, FLU/AZL and AZL/BNZ), respectively. The performed method was efficiently applied to pharmaceutical nasal spray with (mean recoveries ± SD) (99.80 ± 0.97) and (100.26 ± 0.96) for FLU and AZL, respectively. Conclusion: The suggested method was based on simultaneous determination of FLU and AZL in the presence of PEA and BNZ in pure form, laboratory synthetic mixture and its combined pharmaceutical dosage form using green MELC technique with UV detection. The proposed method appeared to be superior to the reported ones of being more sensitive and specific, as well as the separation was achieved with good performance in a relatively short analysis time (less than 7.5 min). Highly acceptable values of LOD and % RSD make this method superior to be used in quality control laboratories with of HPLC technique.

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Determination of N-methyl-2-pyrrolidone and its metabolites in urine by micellar electrokinetic chromatography

Open Chemistry ◽

10.2478/s11532-011-0062-2 ◽

2011 ◽

Vol 9 (5) ◽

pp. 825-833 ◽

Cited By ~ 1

Author(s):

Jana Lokajová ◽

Simo Porras ◽

Eivor Elovaara ◽

Susanne Wiedmer

Keyword(s):

Solid Phase ◽

Background Electrolyte ◽

Sodium Dodecyl ◽

Fused Silica ◽

Rat Urine ◽

Fused Silica Capillary ◽

On Line ◽

Electrokinetic Capillary Chromatography ◽

Silica Capillary

AbstractA fast and accurate micellar electrokinetic capillary chromatography (MEKC) method was developed for monitoring N-methyl-2-pyrrolidone (NMP) exposure. Baseline separation of NMP and its main metabolites: 5-hydroxy-N-methyl-2-pyrrolidone (5HNMP), N-methylsuccinimide (MSI), 2-hydroxy-N-methylsuccinimide (2HMSI), and 2-pyrrolidone (2P) was obtained within 6 min in an uncoated fused silica capillary using 5 mM phosphate buffer and 140 mM sodium dodecyl sulfate (pH 7.1) as background electrolyte (BGE). On-line UV-detection was performed at 200 nm and the applied electric field was 400 V cm−1. Possible interference of BGE-induced system peaks on separation was investigated by computer simulation and no such interference was observed. The developed MEKC method combined with solid phase extraction for sample preparation was successfully applied to the analysis of urine of rats exposed to NMP. The urinary excretion was determined in 0–6 h and 6–24 h specimens collected after an intragastic administration of 308 mg NMP / kg rat body weight. The results of NMP disposition kinetics in rat urine are reported for NMP and metabolites.

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Simultaneous Determination of Ursodeoxycholic Acid and Chenodeoxycholic Acid in Pharmaceutical Dosage Form by HPLC–UV Detection

Journal of AOAC International ◽

10.5740/jaoacint.16-0176 ◽

2017 ◽

Vol 100 (1) ◽

pp. 59-64 ◽

Cited By ~ 1

Author(s):

Mostafa A Khairy ◽

Fotouh R Mansour

Keyword(s):

Ursodeoxycholic Acid ◽

Simultaneous Determination ◽

Chenodeoxycholic Acid ◽

Dosage Form ◽

Reference Method ◽

Reversed Phase ◽

Hplc Method ◽

Uv Detection ◽

Pharmaceutical Dosage Form

Abstract A reversed-phase HPLC method was developed for the simultaneous determination of ursodeoxycholic acid (UDCA) and the epimeric isomer, chenodeoxycholic acid (CDCA), in their synthetic mixtures and in tablet dosage form. The proposed HPLC method uses a C18 column and mobile phase consisting of an acetonitrile–phosphate buffer mixture (pH 2.3, 100 mM; 50 + 50, v/v) at a flow rate of 2.0 mL/min with UV detection at 210 nm. The method was validated according to the International Conference on Harmonization guidelines; and linearity, range,accuracy, precision, robustness,and system suitability were studied. The LOD and LOQ were also calculated and found to be 1.23 and 3.73 μg/mL for UDCA and 0.83 and 2.52 μg/mL for CDCA, respectively. The method was adapted for UHPLC, in which baseline separation was achieved in <2.5 min. The assay results of Ursomix tablets by the developed method were statistically compared with those obtained by the reference method using t- and F-tests, and no significant differences were observed.

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Capillary Electrophoresis Method for Determination of Escitalopram Oxalate in Urine Samples and Different Dosage Forms

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa036 ◽

2020 ◽

Vol 58 (8) ◽

pp. 759-769

Author(s):

Wafa F S Badulla ◽

Arın G Dal Poçan ◽

Zeki Atkoşar ◽

Göksel Arlı

Keyword(s):

Capillary Electrophoresis ◽

Limit Of Detection ◽

Background Electrolyte ◽

Dosage Forms ◽

Fused Silica ◽

Urine Samples ◽

Effective Length ◽

Simple Liquid ◽

Pharmaceutical Dosage Forms

Abstract Application of capillary electrophoresis (CE) has become a rapidly growing analytical technique for the estimation of drugs in pharmaceutical dosage forms and biological fluids. In this study, an effective and sensitive method was developed for the determination of escitalopram oxalate (ESC-OX) by CE with diode-array detection at 200 nm. The separation was achieved by a fused silica capillary with 40 cm effective length (48.5 cm total, 75 μm i.d.). The background electrolyte was composed of 15 mM phosphate buffer (pH 2.5). The applied potential was 22.5 kV, and the samples were injected at 50 mbar pressure for 10 s. Metoprolol was used as an internal standard (IS). The migration time under these optimum conditions was 6.51 ± 0.07 and 6.73 ± 0.08 min for ESC-OX and IS, respectively, with total run time 7 min. The method was validated for linearity, precision, accuracy, specificity and sensitivity. The limit of detection was calculated as 3.85 and 5.07 ng mL−1 for standard and urine samples, respectively. The developed method was employed successfully for the determination of ESC-OX in different pharmaceutical dosage forms and spiked human urine after simple liquid–liquid extraction with good recovery.

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Development of a Micellar Electrokinetic Chromatographic Method with Indirect UV Detection for Pregabalin Determination in Serum Samples

Pharmaceutical Sciences ◽

10.15171/ps.2018.43 ◽

2018 ◽

Vol 24 (4) ◽

pp. 298-303

Author(s):

Hamid Reza Sargazi ◽

Elnaz Tamizi ◽

Elaheh Rahimpour ◽

Abolghasem Jouyban

Keyword(s):

Limit Of Detection ◽

Background Electrolyte ◽

Fused Silica ◽

Uv Detection ◽

Aminosalicylic Acid ◽

Serum Samples ◽

Indirect Uv Detection ◽

Limit Of Quantitation ◽

Fused Silica Capillary

Background: A micellar electrokinetic chromatographic (MEKC)/ indirect UV detection method with hydrodynamic and electrokinetic injection has been developed for the determination of pregabalin in the serum samples. Methods: Separation of the drug was achieved on Agilent capillary electrophorese in less than 5 min using a 50 cm × 75 μm i.d. uncoated fused-silica capillary and a background electrolyte (BGE) consisting of 5-aminosalicylic acid (5-ASA, 10 mmol L-1), cetyl trimethylammonium bromide (CTAB, 1 mmol L-1) and tri-sodium citrate (4% w/v). The influence of various parameters on the separation such as separation voltage, injection time, cassette temperature, pH of BGE and organic modifier was investigated. Results: Method validation shown good linearity (R2> 0.999) in the range of 1.5-100 µg mL-1 of pregabalin. A limit of detection (LOD) of 0.8 μg mL-1 and a limit of quantitation (LOQ) of 2.6 μg mL-1 were reported for pregabalin. Conclusion: The proposed method was found to be suitable and accurate for the determination of pregabalin in serum samples.

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A Rapid Method for Analysis of Phenylalanine in Cereal Products by MEKC-UV Using LC/MS/MS as a Comparative Method

Journal of AOAC International ◽

10.5740/jaoacint.15-052 ◽

2015 ◽

Vol 98 (6) ◽

pp. 1632-1639 ◽

Cited By ~ 2

Author(s):

Andressa Camargo Valese ◽

Luciano Vitali ◽

Roseane Fett ◽

Gustavo Amadeu Micke ◽

Marcone Augusto Leal de Oliveira ◽

...

Keyword(s):

Comparative Method ◽

Background Electrolyte ◽

Sodium Dodecyl ◽

Fused Silica ◽

Migration Time ◽

Effective Length ◽

Cereal Products ◽

Direct Uv Detection ◽

Fused Silica Capillary ◽

Cereal Samples

Abstract The aim of this study was to develop a new and fast micellar electrokinetic chromatography (MEKC) method for the determination of phenylalanine in cereal samples. The background electrolyte was chosen by a factorial design and was composed of 30 mmol/L phosphoric acid, 100 mmol/L sodium dodecyl sulfate, and 25% methanol (v/v) at pH 1.9. A fused silica capillary (48.5 cm total length × 8.5 cm effective length × 50 μm id × 375 μm od) was used in a short-end injection configuration, and direct UV detection was at 200 nm. The method was validated following the Eurachem guidelines, and values such as linearity (from 10.1 to 40.4 mg/L); recovery (86.8–103.9%); repeatability (0.06–0.22% for migration time and 1.14–4.82% for peak area); reproducibility (0.04–0.61% for migration time and 2.22–5.72% for peak area); and LOD and LOQ of 20 and 60 mg/100 g, respectively, were obtained. After the comparison involving selectivity and accuracy between capillary electrophoresis and LC/MS/MS method, the MEKC-UV method was successfully applied to analysis of phenylalanine in different cereal products.

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