scholarly journals Research Article. The Influence of Some Parameters on Chiral Separation of Ibuprofen by High-Performance Liquid Chromatography and Capillary Electrophoresis

2017 ◽  
Vol 63 (1) ◽  
pp. 36-40
Author(s):  
Alina Balint ◽  
Anca Gabriela Cârje ◽  
Daniela Lucia Muntean ◽  
Silvia Imre

Abstract Objective: The aim of the study was to compare the influence of mobile phase composition and temperature on chiral separation of racemic ibuprofen by capillary electrophoresis and high performance liquid chromatography with UV detection. Materials and methods: Racemic ibuprofen was analysed on a chiral OVM column with an HPLC system 1100 Agilent Technologies, under isocratic elution, by using potassium dihydrogen phosphate 20 mM and ethanol in mobile phase. The flow rate was set at 1 mL/min, UV detector at 220 nm and different column temperatures were tested. For electrophoresis separation an Agilent CE G1600AX Capillary Electrophoresis System system, with UV detection, was used. The electrophoresis analysis was performed at different pH values and temperatures, with phosphate buffer 25 mM and methyl-β-cyclodextrin as chiral selector. Results: The chromatograhic analysis reveals a high influence of mobile phase pH on ibuprofen enantiomers separation. An elution with a mixture of potassium dihydrogen phosphate 20 mM pH=3 and ethanol, at 25°C, allowed enantiomers separation with good resolution in less than 8 min. Conclusions: The proposed HPLC method proved suitable for the separation of ibuprofen enantiomers with a good resolution, but the capillary electrophoresis tested parameters did not allow chiral discrimination.

Jurnal MIPA ◽  
2015 ◽  
Vol 4 (2) ◽  
pp. 148
Author(s):  
Lungguk Sitorus ◽  
Julius Pontoh ◽  
Vanda Kamu

Metode HPLC fase terbalik dengan kolom Grace Smart RP 18 5µ dapat digunakan untuk memisahkan dan menentukan konsentrasi asam-asam organik. Metode ini diaplikasikan suhu kolom 40 oC dan dideteksi pada panjang gelombang 210 nm dengan kalium dihidrogenfosfat (pH 2,8) sebagai fase gerak. Metode ini telah digunakan untuk menentukan asam-asam organik seperti asam malat, asam askorbat, asam laktat, asam asetat, asam sitrat, asam piroglutamat, dan asam fumarat.Reverse phase HPLC method using Grace smart RP 18 5µ can used to separating and calculating concentration of organic acid. This method did on 40 0C column temperature and detected on wavelength 210 nm with potassium dihydrogen phosphate (pH 2.8) as mobile phase. Determining of organic acids such as malic acid, ascorbic acid, lactic acid, acetic acid, citric acid, pyroglutamic acid and fumaric acid.


Author(s):  
Choudhary B. ◽  
Goyal A. ◽  
Khokra S. L. ◽  
Kaushik D.

A simple, accurate and reproducible HPLC method have been developed for simultaneous estimation of Diclofenac sodium and rabeprazole from their tablets formulations. A phenomenex C18 (Luna) column of length 250×7.5 mm with particle size of the stationary phase 5 μm and S mobile phase potassium dihydrogen phosphate buffer (pH adjusted to 7.5 with 1 M sodium hydroxide) and acetonitrile in the ratio 60: 40 were used in this study. Retention time was found to be 9.20 min and 6.40 min for Rabeprazole and diclofenac sodium respectively. While that for internal standard as domperidone was 11.87 min at a flow rate of 2ml / min. Linearity was found in the concentration range of 10-50 μg /ml for both the drugs in this method. The results of analysis have been validated statistically and also by recovery studies.


Author(s):  
Hossein Salmanizadeh ◽  
Neda Sahi

Argininosuccinic aciduria is an autosomal, recessive amino acid disorder that is caused by a deficiency of the argininosuccinate lyase enzyme. Citrulline is the most significant marker to detect this disorder. We used the High-performance liquid chromatography with fluorescence detection with 450 nm emission and 330 nm excitation wavelengths, 15 mmol/L potassium dihydrogen phosphate and 5 mmol/L dipotassium hydrogen phosphate as Mobile Phase A, and 50 mL water, 250 mL acetonitrile, and 200 mL methanol as Mobile Phase B in gradient mode with flow rate of 1.2 mL/min. The citrulline concentration was 22 µmol/L in healthy infants and 220 µmol/L in infants suffering from the disorder.


2007 ◽  
Vol 90 (6) ◽  
pp. 1573-1578 ◽  
Author(s):  
Charmy R Shah ◽  
Nehal J Shah ◽  
Bhanubhai N Suhagia ◽  
Natvarlal M Patel

Abstract This paper describes validated high-performance liquid chromatographic (LC) and high-performance thin-layer chromatographic (TLC) methods for the simultaneous estimation of olanzapine and fluoxetine in pure powder and tablet formulations. The LC separation was achieved on a Lichrospher 100 RP-180, C18 column (250 mm, 4.0 mm id, 5 m) using 0.05 M potassium dihydrogen phosphate buffer (pH 5.6 adjusted with o-phosphoric acid) acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1 mL/min and ambient temperature. The TLC separation was achieved on aluminum sheets coated with silica gel 60F254 using methanoltoluene (40 + 20, v/v) as the mobile phase. Quantitation was achieved by measuring ultraviolet absorption at 233 nm over the concentration range of 1070 and 40280 g/mL with mean recovery of 99.54 0.89 and 99.73 0.58% for olanzapine and fluoxetine, respectively, by the LC method. Quantitation was achieved by measuring ultraviolet absorption at 233 nm over the concentration range of 100800 and 4003200 ng/spot with mean recovery of 101.53 0.06 and 101.45 0.35% for olanzapine and fluoxetine, respectively, by the TLC method with densitometry. These methods are simple, precise, and sensitive, and they are applicable for simultaneous determination of olanzapine and fluoxetine in tablet formulations.


2010 ◽  
Vol 93 (1) ◽  
pp. 97-101
Author(s):  
Michal Douša ◽  
Michaela Dubovská

Abstract A rapid procedure based on a direct extraction and HPLC determination of dihydroergocristine in a pharmaceutical preparation with fluorescence detection has been developed and validated. The optimized chromatographic conditions included a Purospher RP18e column, 5 µm particle size, 250 4.0 mm, and 25 mM potassium dihydrogen phosphate buffer (pH 2.8)acetonitrile (60 + 40, v/v) mobile phase at a flow rate of 1 mL/min. The separation was carried out at 50C, and the injection volume was 5 L. Fluorescence detection was performed at an excitation and emission wavelength of 224 and 344 nm, respectively. The mobile phase parameters such as organic solvent composition, temperature, and pH were studied. The proposed method has the advantages of a very simple sample pretreatment and fast HPLC determination.


2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Laura D. Simionato ◽  
Leonardo Ferello ◽  
Sebastián Stamer ◽  
Patricia D. Zubata ◽  
Adriana I. Segall

Simple, sensitive, and economical simultaneous volumetric and HPLC methods for the determination of pridinol mesylate in raw material have been developed. The volumetric method is based on the reaction of pridinol with sodium lauryl sulphate in diluted sulphuric acid. Dimethyl yellow was used as indicator to detect the end point of the titration in aqueous/organic layer. The HPLC method for the determination of pridinol mesylate employs a reverse phase C18 column at ambient temperature with a mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate, pH adjusted to 5.0 (1 : 2, v/v). The flow rate was 0.8 mL/min. Quantitation was achieved with UV detection at 258 nm based on peak area. Both methods were found to be suitable for the quality control of pridinol mesylate in raw material.


Author(s):  
Dinh Hai Le ◽  
Thu Nguyen Thi ◽  
Trang Vu Thi ◽  
Thuy Le Thi ◽  
◽  
...  

This study aimed to develop a HPLC method to simultaneously analyze guanosine 5’-monophosphat (GMP) and inosine 5’-monophosphat (IMP) in food products. Sample preparation procedure was simple, fast. A C18 column (250 mm × 4.6 mm, 5 µm) was used as stationary phase, and a mixture of 10 mM potassium dihydrogen phosphate and 5 mM sodium heptanesulfonate was applied as mobile phase, and PDA detector at 250 nm. The method validation followed AOAC criteria. Selectivity, linearity (R2 > 0.999), recovery (IMP: 90.5 % - 102.8 %, GMP: 91.5 % - 103.9 %), repeatability (RSDR of IMP: 3.07 % and GMP: 2.83 %) were acceptable to determination GMP and IMP in food matrix under AOAC guidelines. LOD of GMP and IMP were of 2.32 and 2.77 mg/kg, respectively. This method was used to determination GMP, IMP in food products collected in Hanoi markets.


Author(s):  
Bhoomi Dineshkumar Patel ◽  
Nidhi J. Dharsandiya ◽  
Ankit Chaudhary

The objective of the study is a simple, precise and accurate stability RP-HPLC method has been developed and subsequently validated for the estimation of Teneligliptin and its impurity in tablet formulation. The adequate separation was carried out using Grace Smart C18 column (250mm x 4.6mm, 5?m particle size), mixture of 0.05M Potassium dihydrogen phosphate PH 4.0 and Acetonitrile 80:20 % v/v as a mobile phase with a flow rate of 1 ml/min and the effluent was monitored at 242 nm using PDA detector. The retention time of Teneligliptin, Impurity B and Impurity G were 7.443 min, 6.650 min and 8.473 min respectively. Linearity for Teneligliptin, Impurity B and Impurity G were found in the range of 500-3000 µg/ml (R2 = 0.998), 5-15 µg/ml (R2 = 0.994) and 5-15 µg/ml (R2 = 0.998) respectively. The accuracy of the present method was evaluated at 50%, 100% and 150%. The % recoveries of drug were found to be in range of 99.315 ± 0.283 for Teneligliptin. Precision studies were carried out and the RSD values were less than two. The method was found to be robust. The proposed method was found to be specific, accurate, precise and robust can be used for simultaneous estimation of these drugs in tablet dosage form.


1999 ◽  
Vol 82 (2) ◽  
pp. 248-250 ◽  
Author(s):  
Yuzo Yamamoto ◽  
Fusao Kondo

Abstract A high-performance liquid chromatographic (HPLC) method for determining glycarbylamide (GB) in chicken tissue was developed. GB was extracted with acetonitrile, followed by solid-phase extraction cleanup using a Bond Elut cartridge column with neutral alumina. After the extract had been evaporated to dryness, the residue was dissolved in 1.0 mL 0.1 N sodium hydroxide. Then 1.0 mL 0.1 M potassium dihydrogen phosphate solution was added to it. HPLC separation was done on a 250 × 4.6 mm id TSK-GEL ODS 80™TM column with 0.05M potassium dihydrogen phosphate as the mobile phase. Ultraviolet detection was done at a wavelength of 260 nm. The calibration curve of standard GB solutions was linear between 0.16 and 3 μg/mL (correlation coefficient, r = 0.999). The recovery of GB from chicken muscle spiked at 0.8 μg/g was 88.6 ± 2.3% (mean ± standard deviation, n = 5), and the lower limit of determination was 0.05 μg/g in chicken muscle.


Author(s):  
Sumithra Sumithra ◽  
Shanmugasundaram P ◽  
Ravichandiran V

ABSTRACTObjective: Innovative application of quality by design (QbD) technique for simultaneous estimation of levofloxacin and ambroxol hydrochloride (HCL)in bulk and its pharmaceutical dosage form using reverse phase-high-performance liquid chromatography (RP-HPLC) method.Method: A method has been developed for the separation of levofloxacin and ambroxol HCL using RP-HPLC on C18 column (250 4.6 mm, 5 ml) withultraviolet detection at 306 nm. Experimental designs were applied for multivariate optimization of the experimental conditions of RP-HPLC method.Three independent factors: Acetonitrile content in the mobile phase composition, buffer pH, and flow rate were used to design mathematical models.Here, central composite design (CCD) experimental design was used to study the response surface technique and to study in depth the effects ofthese independent factors. Derringer’s desirability function was applied to simultaneously optimize the retention time of last eluting peak (ambroxolhydrochloride) and resolution between levofloxacin and ambroxol hydrochloride.Result and Discussion: The predicted optimum assay condition consisted of acetonitrile, potassium dihydrogen phosphate buffer (pH 5.00;potassium dihydrogen phosphate), and methanol in a proportion of 20:70:10% v/v, respectively, as the mobile phase at a flow rate of 1.2 ml/minute.Using this optimum condition, baseline separation of both drugs with good resolution and a run time of <5 minutes were achieved. The optimizedassay condition was validated according to the ICH guidelines to confirm specificity, linearity, accuracy, and precision.Keywords: Levofloxacin, Ambroxol hydrochloride, Experimental design, Response surface methodology, Derringer’s desirability, Quality by designapproach.


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