scholarly journals Simultaneous determination of amlodipine and telmisartan from pharmaceutical products by way of capillary electrophoresis

2016 ◽  
Vol 29 (1) ◽  
pp. 42-46 ◽  
Author(s):  
Adriana Modroiu ◽  
Gabriel Hancu ◽  
Robert Alexandru Vlad ◽  
Ștefana Stăcescu ◽  
Ruxandra Soare ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Applied Voltage ◽  
Limit Of Detection ◽  
Pharmaceutical Products ◽  
Fused Silica ◽  
Fixed Dose ◽  
Array Detector ◽  
System Temperature ◽  
Fused Silica Capillary

AbstractA rapid, simple and sensitive capillary zone electrophoresis method was developed for the simultaneous determination of amlodipine besylate and telmisartan, in fixed-dose combinations, through the utilization of a UV photodiode array detector. Electrophoretic parameters such as buffer concentration and pH, system temperature, applied voltage and injection parameters, were optimized in order to improve the efficiency of the separation. The best results were obtained when employing fused silica capillary (48 cm length X 50 μm ID) and 50 mM phosphate buffer electrolyte at pH 4.50, + 25 kV applied voltage, as well as 25°C system temperature. The separation was achieved in approximately 3 minutes, with a resolution of 4.90, while the order of migration was amlodipine followed by telmisartan. The analytical performance of the method was verified with regard to linearity, precision and robustness. In addition, the limit of detection and the quantification were calculated.

Application of MEKC and UPLC with Fluorescence Detection for Simultaneous Determination of Amlodipine Besylate and Bisoprolol Fumarate

2020 ◽  
Author(s):  
Sohila M Elonsy ◽  
Fawzy A El Yazbi ◽  
Rasha A Shaalan ◽  
Hytham M Ahmed ◽  
Tarek S Belal
Keyword(s):  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
Fused Silica ◽  
Effective Length ◽  
Fixed Dose ◽  
Array Detector ◽  
Internal Diameter ◽  
Amlodipine Besylate ◽  
Validation Parameters

Abstract Objective Two chromatographic methods were described for simultaneous determination of the antihypertensive drugs amlodipine besylate (AML) and bisoprolol fumarate (BIS). Methods Method I applies micellar electrokinetic capillary chromatography using a deactivated fused silica capillary (25 cm effective length × 50 μm internal diameter). The background electrolyte consisted of 0.01 M borate buffer (pH 9.2) containing 0.025 M sodium dodecyl sulphate and methanol in the ratio of 80:20 (v/v). Valsartan (VAL) was used as an internal standard. Diode array detector was set at 238, 224, and 210 nm for measuring AML, BIS, and VAL, respectively. Method II involves using ultra-performance liquid chromatography with fluorescence detection. Zorbax SB-C8 column (2.1 × 100 mm, 1.8 μm particle size) was used with isocratic elution of the mobile phase composed of 0.1% trifluoroacetic acid, acetonitrile, and methanol in the ratio of 55:35:10 (v/v) at a flow rate of 0.6 mL/min. Fluorescence detection was done using excitation wavelengths 230 and 370 nm and emission wavelengths 305 and 450 nm for BIS and AML, respectively. Validation parameters were carefully studied including linearity, ranges, precision, accuracy, robustness, detection, and quantification limits. Results Method I showed good linearity over the range 10–100 μg/mL for both dugs. Method II’s linear ranges were 0.001–0.1 and 0.02–1 µg/mL for BIS and AML, respectively. Conclusion The proposed methods were successfully validated and applied for assay of the studied drugs in their fixed-dose combination tablets. Highlights To the best of our knowledge, this study suggests the first electro-chromatographic and LC with fluorescence detection methods for simultaneous determination of amlodipine and bisoprolol.

Development and Validation of an HPLC Method for Simultaneous Determination of Rifampicin, Isoniazid, Pyrazinamide, and Ethambutol Hydrochloride in Pharmaceutical Formulations

2015 ◽  
Vol 98 (5) ◽  
pp. 1234-1239 ◽  
Author(s):  
Paula R Chellini ◽  
Eduardo B Lages ◽  
Pedro H C Franco ◽  
Fernando H A Nogueira ◽  
Isabela C César ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Combined Treatment ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Fixed Dose Combination ◽  
Fixed Dose ◽  
Array Detector ◽  
Equilibration Time ◽  
Dose Combination

Abstract Tuberculosis treatment consists of a fixed dose combination of rifampicin (RIF), isoniazid (INH), pyrazinamide (PYZ), and ethambutol hydrochloride (EMB). The combined treatment using various drugs is necessary for patient curing, without recrudescence, and for prevention of drug-resistant mutants, which may occur during treatment. An HPLC-diode array detector (DAD) method for the simultaneous determination of RIF, INH, PYZ, and EMB in fixed dose combination tablets was developed and validated. Chromatographic experiments were performed on an Agilent 1200 HPLC system, and the separation was carried out on a Purospher STAR RP18e (250 × 4.6 mm id, 5 μm, Merck) analytical column. Gradient elution was carried out with a mobile phase of 20 mM monobasic sodium phosphate buffer with 0.2% triethylamine (pH 7.0) and acetonitrile at a flow rate of 1.5 mL/min. The total run time was 12 min, and the re-equilibration time was 5 min. EMB detection was performed at 210 nm, and RIF, INH, and PYZ were detected at 238 nm, using a DAD. The method proved to be specific, linear (r2 > 0.99), precise (RSD <2%), accurate, and robust and may be applied to the QC analysis of pharmaceutical formulations.

Simultaneous Multiresidue Analysis of (β-Lactam Antibiotics in Bovine Milk by Liquid Chromatography with Ultraviolet Detection and Confirmation by Electrospray Mass Spectrometry

1994 ◽  
Vol 77 (5) ◽  
pp. 1122-1131 ◽  
Author(s):  
Krystyna L Tyczkowska ◽  
Robert D Voyksner ◽  
Rolf F Straub ◽  
Arthur L Aronson
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Electrospray Mass Spectrometry ◽  
Limit Of Detection ◽  
Water Solution ◽  
Bovine Milk ◽  
Penicillin G ◽  
Array Detector

Abstract A multiresidue analytical method was developed for the simultaneous determination of amoxicillin, cephapirin, procaine penicillin G, ampicil-lin, cloxacillin, and ceftiofur in bovine milk. The method involved ultrafiltration of milk diluted with an equal volume of 50% acetonitrile through a 10 000 dalton molecular mass cutoff filter. Separation of these β-lactam antibiotics from other milk components was performed by ion-paired (octane- and dodecanesulfonate) liquid chromatography using a phenyl column eluted with acetonitrile-water solution. Ultraviolet ab-sorbance of the column effluent was monitored in the 200-350 nm range of a photodiode-array detector. For quantitation, the chromatograms were acquired at λ210 nm for penicillin G, am-picillin, and cloxacillin; λ230 nm for amoxicillin; and λ290 for cephapirin, procaine, and ceftiofur. The limit of detection for the simultaneous determination of these antibiotics was estimated to be 100 ppb. Liquid chromatography/electrospray mass spectrometry could be used to confirm these antibiotics for quantities down to 100 pg entering the mass spectrometer.

scholarly journals Simultaneous Determination of Some Active Ingredients in Cough and Cold Preparations by Gas Chromatography, and Method Validation

2005 ◽  
Vol 88 (4) ◽  
pp. 1093-1098 ◽  
Author(s):  
Thresiana Harsono ◽  
Mochammad Yuwono ◽  
Gunawan Indrayanto
Keyword(s):  
Simultaneous Determination ◽  
Fused Silica ◽  
Chlorpheniramine Maleate ◽  
Column Temperature ◽  
Flame Ionization ◽  
Phenylpropanolamine Hydrochloride ◽  
Fused Silica Capillary ◽  
Silica Capillary Column ◽  
Dextromethorphan Hydrobromide

Abstract A simple and rapid gas chromatographic (GC) method has been developed for the simultaneous determination of combinations of acetaminophen, phenylpropanolamine hydrochloride, guaifenesin, pseudoephedrine hydrochloride, caffeine, chlorpheniramine maleate, and dextromethorphan hydrobromide in cough and cold tablets and syrups. After extraction of the analyte with alkaline ethyl acetate, 2 μL extract was injected (splitting ratio of 50:1) into a gas chromatograph equipped with a CBP1-M25-025 fused silica capillary column (25 m × 0.22 mm; film thickness, 0.25 μm). The column temperature was held at 150°C for 5 min, increased to 175°C at 3°C/min, and increased to 270°C at 10°C/min. The temperatures of the flame ionization detector and injector were maintained at 300°C. The GC method is inexpensive, rapid, accurate, and precise, and thus it can be used for routine analysis of tablet and syrup preparations in quality control laboratories of pharmaceutical companies.

scholarly journals Development and validation of an HPLC method for the simultaneous determination of artesunate and mefloquine hydrochloride in fixed-dose combination tablets

2013 ◽  
Vol 49 (4) ◽  
pp. 837-843 ◽  
Author(s):  
Fernando Henrique Andrade Nogueira ◽  
Naialy Fernandes Araújo Reis ◽  
Paula Rocha Chellini ◽  
Isabela da Costa César ◽  
Gerson Antônio Pianetti
Keyword(s):  
Simultaneous Determination ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Fixed Dose Combination ◽  
Fixed Dose ◽  
Array Detector ◽  
Control Analysis ◽  
Dose Combination ◽  
Development And Validation

The present study developed and validated an HPLC method for the simultaneous determination of artesunate (AS) and mefloquine hydrochloride (MQ) in fixed-dose combination tablets, according to ICH guidelines. The chromatographic separation was carried out on an XBridge C18 (250 x 4.6 mm i.d., 5 µm particle size, Waters) analytical column. The mobile phase included a 0.05 M monobasic potassium phosphate buffer (pH adjusted to 3.0 with phosphoric acid) and acetonitrile (50 + 50, v/v). The flow rate was 1.0 mL/min, and the run time was 13 minutes. A dual-wavelength approach was employed: AS detection was performed at 210 nm and MQ was detected at 283 nm, using a diode array detector. Stability of sample solutions was evaluated for 8 hours after preparation, during which time the solutions remained stable. Youden's test was employed to evaluate robustness. The method proved to be linear (r²>0.99), precise (RSD<2.0%), accurate, selective, and robust, proving to be appropriate for routine drug quality control analysis.

Validated Stability-Indicating Capillary Electrophoresis Method for the Separation and Determination of a Fixed-Dose Combination of Carvedilol and Hydrochlorothiazide in Tablets

2013 ◽  
Vol 96 (5) ◽  
pp. 951-959 ◽  
Author(s):  
Nourah Z Alzoman ◽  
Maha A Sultan ◽  
Hadir M Maher ◽  
Mona M AlShehri ◽  
Ileana V Olah
Keyword(s):  
Capillary Electrophoresis ◽  
Degradation Products ◽  
Background Electrolyte ◽  
Internal Standard ◽  
Fused Silica ◽  
Fixed Dose ◽  
Array Detector ◽  
Forced Degradation ◽  
Stability Indicating

Abstract A novel, fast, sensitive, and specific capillary electrophoresis (CE) technique coupled to a diode array detector has been developed for the separation and simultaneous determination of carvedilol (CRV) and hydrochlorothiazide (HCT) in two combination formulations. The proposed method utilized a fused silica capillary (55 cm × 75 μm id) and the background electrolyte solution phosphate buffer (12.5 mM, pH 7.4)–methanol (95 + 5, v/v). The separation was achieved at 30 kV applied voltage and 24°C. Atorvastatin (80 μg/mL) was chosen as the internal standard. The described method was linear over the range of 1–200 and 0.2–150 μg/mL for CRV and HCT, respectively. Intraday and interday RSD (n = 6) was ≤1.4%. The LOD values of CRV and HCT were 0.26 and 0.07 μg/mL, respectively. The validated CE method was successfully applied to the analysis of two commercial tablet dosage forms. Forced degradation studies were performed on bulk samples of the two drugs using thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation products produced as a result of stress studies did not interfere with the determination of CRV and HCT; the assay could, therefore, be considered stability-indicating.

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

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.

Simultaneous Determination of D- and L-Malic Acids in Apple Juice by Gas Chromatography

1988 ◽  
Vol 71 (3) ◽  
pp. 466-468 ◽  
Author(s):  
Vipin K Agarwal
Keyword(s):  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Apple Juice ◽  
Capillary Column ◽  
Butyl Ester ◽  
Fused Silica ◽  
Fused Silica Capillary ◽  
Silica Capillary Column ◽  
Silica Capillary

Abstract A gas chromatographic (GC) method was developed for the simultaneous determination of D- and L-malic acids in apple juice. D-Malic- (R)-(-)-2-butyl ester and L-malic-(R)-(-)-2-butyl ester are prepared with (R)-(-)-2-butanol. These diastereomers are separated and quantitated by gas chromatography on a Carbowax 20M (30 m x 0.25 mm) fused silica capillary column. This procedure does not involve any extraction or cleanup step.

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