scholarly journals Determination of Folic Acid in Multivitamin Preparations by Reversed Phase HPLC

2021 ◽  
Vol 11 (3) ◽  
pp. 185-192
Author(s):  
A. S. Alekseeva ◽  
M. V. Gavrilin ◽  
T. B. Shemeryankina ◽  
M. S. Smirnova ◽  
E. P. Fedorova ◽  
...  
Keyword(s):  
Folic Acid ◽  
Silica Gel ◽  
Ferrous Sulfate ◽  
Reversed Phase ◽  
Asymmetry Factor ◽  
Array Detector ◽  
Isocratic Elution ◽  
Rp Hplc ◽  
Acid Determination

A great variety of components in multivitamin preparations containing folic acid, and a variety of test methods and conditions of folic acid determination proposed by manufacturers, require alignment of test procedures for products with similar composition.The aim of the study was to compare the results of experimental verification of folic acid determination procedures which use reversed phase high-performance liquid chromatography (RP HPLC) with isocratic elution mode. Materials and methods: The Agilent 1260 Infinity II LC system with a diode array detector (280 nm), isocratic elution mode, C8- and C18-bonded silica gel chromatographic columns, model mixtures containing folic acid, cyanocobalamin, ferrous sulfate, and potassium iodide, were used in the study.Results: The lowest relative standard deviation of the folic acid peak area (RSD=0.09%), and the lowest asymmetry factor (As=1.04) for folic acid were observed for the model mixture “ferrous sulfate+folic acid+cyanocobalamin” and the following test conditions. Column: 250×4.0 mm, silica gel for chromatography, octylsilyl (C8), endcapped; mobile phase:  methanol‒phosphate buffer (12:88), pH 6.6; column temperature: 25ºС. The study demonstrated the feasibility of using these conditions for determination of pteroic acid impurity with simultaneous precipitation of interfering ferrous ions, using ethylenediaminetetraacetic acid solution, pH 9.5, as a solvent.Conclusions: RP HPLC can be recommended as an optimal aligned test procedure for determination of folic acid in combination products. It is recommended to use a solution containing folic and pteroic acids for system suitability testing.

Validated Chromatographic and Spectrofluorimetric Methods for Analysis of Silodosin: A Comparative Study with Application of RP-HPLC in the Kinetic Investigation of Silodosin Degradation

2020 ◽  
Author(s):  
Shereen A Boltia ◽  
Mohammed Abdelkawy ◽  
Taghreed A Mohamed ◽  
Nahla N Mostafa
Keyword(s):  
Analytical Methods ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Array Detector ◽  
Kinetic Investigation ◽  
First Derivative ◽  
Rp Hplc ◽  
Significant Difference

Abstract Background Stability indicating determination of pharmaceuticals is crucial, especially for drugs which have few published official analytical methods. Silodosin (SLD) is an FDA approved α1A-adrenoceptor blocker. Objective Efficient analytical methods were suggested, based on different instrumental techniques for quantification of SLD, besides conducting kinetic investigation of its degradation. Methods The first method is based on Reversed Phase High Performance Liquid Chromatography with Photodiode Array Detector (RP-HPLC-PDAD). Detection is done at wavelength 225 nm. The second method is focused on using High Performance Thin Layer Chromatography (HPTLC) and eluting the drug by solvent mixture followed by scanning at wavelength 270 nm. The third method depends on the First Derivative Synchronous Fluorescence Spectroscopy (1DSFS) for analysis of solutions of SLD and its acid and oxidative induced degradation products at Δλ = 90 nm, then determining the first derivative of the spectra and measuring peak amplitudes at 360 nm. Results Acceptable linearities were found in the concentration range of 0.50–90 μg/mL, 0.10–3.0 μg/band, and 0.05–0.50 µg/mL, for RP-HPLC-PDAD, HPTLC, and spectrofluorimetric methods, respectively. Conclusion Statistical analysis showed no significant difference between the suggested and the reported method. In monitoring the kinetics of SLD degradation, the order of reactions was determined and effects of degrading agent concentration and temperature on reaction rate were studied. Highlights Three analytical methods were developed for the determination of SLD based on RP-HPLC-PDAD, HPTLC, and 1DSFS in bulk and capsule dosage form. In addition, kinetic investigation of SLD degradation was performed using the developed RP-HPLC-PDAD method.

scholarly journals A Validated RP-HPLC Method for the Determination of Butamirate Citrate and Benzoic Acid in Syrup, Based on an Experimental Design Assessment of Robustness

Separations ◽  
2021 ◽  
Vol 8 (10) ◽  
pp. 163
Author(s):  
Antonios-Dionysios G. Neofotistos ◽  
Kostas Gkountanas ◽  
Haris Boutsikaris ◽  
Yannis Dotsikas
Keyword(s):  
Experimental Design ◽  
Benzoic Acid ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Buffer Solution ◽  
Solution Ph ◽  
Design Assessment ◽  
Rp Hplc

A reversed-phase high-pressure liquid chromatography (RP-HPLC) method was developed and subsequently validated for the simultaneous determination of butamirate citrate (BC) and benzoic acid (BA) in cough syrup. The separation was performed employing a cyanopropyl column with a mobile phase consisting of 50%/50% v/v MeOH/NaH2PO4 * H2O 50 mM aqueous solution pH = 3.0. The quantitation was achieved with a diode array detector (DAD) at 210 nm. The method demonstrated a congenitally satisfactory separation, yet the acquired peaks were asymmetrical. This effect was eliminated by using 1% triethylamine in the buffer solution as a silanol blocker. In addition, the method was found to unequivocally assess the target analytes in the sample matrix and fulfilled the required specifications in relevance to specificity, linearity, accuracy, precision and stability of both the standard solutions and of the sample solutions. Lastly, an experimental design was designed in order to assess the robustness of the proposed assay. To this purpose, a graphical and a statistical approach were utilized and compared to identify the factors that should be strictly controlled during each execution of the method.

Simultaneous Determination of Co-administrated Deflazacort, Aprepitant and Granisetron in Dosage Forms and Spiked Human Plasma by RP-HPLC/PAD

2019 ◽  
Vol 57 (9) ◽  
pp. 790-798 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Soheir Alweshahy ◽  
Dalia A Elshabasy ◽  
Nadia F Youssef
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Array Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array

Abstract A selective reversed phase high performance liquid chromatography/photodiode array detector (RP-HPLC/PAD) method has been developed for simultaneous determination of the three co-administrated deflazacort, aprepitant and granisetron drugs used with chemotherapy. The three cited drugs have been chromatographed on C18 column using a mobile phase consisting of acetonitrile–0.2% v/v triethylamine (80:20 v/v, pH of 6.6 ± 0.05) with isocratic elution and monitored by photodiode array at 220 nm. International conference on harmonization (ICH) guidelines were followed to validate the developed method. Successful application of the developed method was assessed by the simultaneous determination of the studied drugs in pure forms, dosage forms and plasma samples in the ranges of 0.2–20, 0.4–40 and 0.2–20 μg/mL for deflazacort, aprepitant and granisetron, respectively.

scholarly journals RP-HPLC method with indirect UV detection for determination of sodium ibandronate in pharmaceuticals

2019 ◽  
Vol 64 (02) ◽  
pp. 43-49
Author(s):  
Zharko Tanturovski ◽  
Zorica Arsova-Sarafinovska ◽  
Aneta Dimitrovska
Keyword(s):  
Sodium Salt ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Array Detector ◽  
Ibandronic Acid ◽  
Indirect Uv Detection ◽  
Rp Hplc

Ibandronate sodium (IBN) [(1-hydroxy-3- (methyl pentyl amino) propylidene bisphosphonic acid monosodium monohydrate)] is the sodium salt of ibandronic acid, a synthetic nitrogen-containing bisphosphonate drug. The aim of this study was to develop a sensitive and accurate RP-HPLC method with indirect UV detection for determination of IBN in pharmaceutical formulations. Chromatographic separation was performed on a Waters Bridge C18 reversed-phase column (250 x 4.6 mm I.D.; particle size 5 µm), in an isocratic mode with a mobile phase constituted of 90% buffer: 10% acetonitrile (V/V). The buffer was made using 1.5 mL ortho-phosphoric acid, 990 mg 1-Hexanesulfonic acid sodium salt 98%, 140 mg EDTA in 1000 mL flask diluted with HPLC grade water. The elution was carried out at a flow rate of 1.0 mL minˉ1. A diode array detector measured the UV absorbance at 198 nm, in inverse mode. The method was validated for specificity/selectivity, linearity, LOD, LOQ, accuracy, precision and robustness according to ICH validation guidelines. The limits of detection and quantification were calculated at 0.0163 µg/mL and 0.0495 µg/mL, respectively. The method was effectively used for determination of IBN from commercial tablets and provided good results without any interference from commonly used excipients. Keywords: RP-HPLC with indirect UV detection, Ibandronate sodium, validation, pharmaceuticals

scholarly journals DEVELOPMENT OF METHODS OF PRE-COLUMNAR DERIVATIZATION OF GLUTATHIONES RECOVERED BY 4-METHOXY-2-NITROPHENYLISOTHIOTOCIONATE FOR DETERMINATION BY METHOD OF HIGH-EFFECTIVE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 6 (3) ◽  
pp. 229-240
Author(s):  
K. A. Alexeeva ◽  
D. I. Pisarev ◽  
O. O. Novikov ◽  
A. Yu. Malyutina
Keyword(s):  
High Performance ◽  
Uv Light ◽  
Heart Diseases ◽  
Spectral Characteristics ◽  
Analytical Signal ◽  
Direct Analysis ◽  
Reversed Phase ◽  
Array Detector ◽  
Rp Hplc

Nowadays the pharmacological role of glutathione in the therapy of carcinogenesis, neurodegenerative and ocular diseases, heart diseases, the immune system and aging of the organism is being actively investigated. Therefore, for the development of pharmaceutical medical forms on its basis, it is necessary to create an optimal analytical base. The aim of this study is to develop a methodology for the analysis of glutathione recovered by pre-columnar derivatization of 4-methoxy-2-nitrophenyl isothiocyanate. Materials and methods. Since glutathione does not have the necessary spectral characteristics for its direct analysis, a methodology for the determination of glutathione with the use of pre-columnar derivatization of 4-methoxy-2-nitrophenyl-isothiocyanate by reversed-phase high-performance chromatography (RP HPLC) has been developed on that basis. Detection of the resulting derivative has been carried out by absorption in UV light using a diode array detector. Results and discussion. In the course of the experiment described, chromatograms of a glulathione derivative with 4-methoxy-2-nitrophenyl isothiocyanate were obtained. This technique was also evaluated for the possibility of quantitative determination of glutathione. The sensitivity of the methods was 0.01% or 3.1*10-1 mol. The linear relationship between the analytical signal (peak area) and concentration was observed within the range of 0.01–0.08% and the correlation coefficient of 0.995. Conclusion. In the course of the studies, a methodology for the determination of glutathione has been developed with the use of pre-columnarderivatization of 4-methoxy-2-nitrophenyl-isothiocyanate by RP HPLC. In this case, the derivative is formed with the retention time of 22.3 minutes and the absorption maximum of 398 nm. This method also allows estimating the quantitative content of the object under study.

scholarly journals Optimization and validation of a derivatization method for analysis of biogenic amines in wines using RP-HPLC-DAD

2016 ◽  
Vol 35 (1) ◽  
pp. 19 ◽  
Author(s):  
Krste Tashev ◽  
Violeta Ivanova-Petropulos ◽  
Marina Stefova
Keyword(s):  
Biogenic Amines ◽  
High Performance ◽  
Standard Addition ◽  
Reversed Phase ◽  
Array Detector ◽  
Red Wines ◽  
Rp Hplc ◽  
Good Repeatability ◽  
Repeatability And Reproducibility

An analytical method for determination of the biogenic amines: tryptamine, putrescine  histamine, phenylethylamine, tyramine, cadaverine, spermidine and spermine in red and white wines using pre-column derivatization with dansyl chloride (DnsCl) and reversed phase-high performance liquid chromatography with diode array detector (RP-HPLC-DAD) was developed and optimized. Concentration of DnsCl, pH, time of reaction and evaporation under nitrogen were tested and optimized. Best recoveries, ranging from 72 to 102 % were obtained for all analyzed amines applying derivatization with 10 mg/mL of DnsCl for 1 h at 60 oC and pH 9. The developed method showed excellent linearity with R2>0.99 for all tested amines. The accuracy was checked with the standard addition method showing satisfactory recovery, good repeatability and reproducibility. The optimized and validated method was applied for analysis of white and red wines from Macedonian origin, observing higher total amounts of biogenic amines in red wines. 

scholarly journals RP-HPLC determination of vitamins, folic acid and B12 in multivitamin tablets

2005 ◽  
Vol 70 (10) ◽  
pp. 1229-1235 ◽  
Author(s):  
Rada Amidzic ◽  
Jasmina Brboric ◽  
Olivera Cudina ◽  
Sote Vladimirov
Keyword(s):  
Folic Acid ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pyridoxine Hydrochloride ◽  
Statistical Parameters ◽  
Rp Hplc ◽  
Acid Sodium Salt ◽  
Multivitamin Preparation

A simple and sensitive reversed-phase, ion-pair HPLC method was developed and validated for the simultaneous determination of B-group vitamins, thiamine chloride hydrochloride (B1), nicotinamide (B3), pyridoxine hydrochloride (B6) and folic acid in Pentovit? coated tablets. The cyanocobalamine (B12) was determined separately, because of its low concentration in the investigated multivitamin preparation. RP-HPLC analysis was per- formed with a LKB 2150 HPLC system, equipped with a UV/VIS Waters M 484 detector. The procedures for the determination of B1, B2, B6 and folic acid were carried out on a Supelcosil ABZ+ (15 cm 4.6 mm; 5 m) column with methanol-5mM heptanesulphonic acid sodium salt 0.1 % triethylamine TEA (25:75 V/V); pH 2.8 as the mobile phase. For the determination of B12 a Suplex pKb-100 (15 cm 4.6 mm; 5 m) column and methanol?water (22:78 V/V) as the mobile phase were used. The column effluents were monitored at 290 nm for B1, B3, B6 and folic acid, and at 550 nm for B12. The obtained results and statistical parameters for all the investigated vitamins of the B-group in Pentovit? coated tablets were satisfactory and ranged from 90.4 % to 108.5 % (RSD. from 0.5 % to 4.1 %). The parameters for the validation of the methods are given.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

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