scholarly journals Quantitation of artemether in pharmaceutical raw material and injections by high performance liquid chromatography

2009 ◽  
Vol 45 (4) ◽  
pp. 737-742 ◽  
Author(s):  
Isabela da Costa César ◽  
Gerson Antônio Pianetti
Keyword(s):  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Raw Material ◽  
Ultraviolet Detection ◽  
Injection Volume ◽  
Routine Quality Control

The quantitation of artemether in both pharmaceutical raw material and injections was carried out by high performance liquid chromatography (HPLC) with ultraviolet detection. A Zorbax C18 column (150 x 4.6 mm; 5 μm), at 30 °C, and a mobile phase composed of acetonitrile and water (70:30), at a flow rate of 1ml/min, were used. The detection wavelength was 216 nm and the injection volume was 20 μL. The method proved to be linear (r²=0.9999), precise (RSD < 20% for intra-day and inter-day precision), accurate and selective regarding possible impurities and excipients of the samples. The detection and quantitation limits were 8 μg/mL and 25 μg/mL, respectively. The artemether content obtained in the raw material analysis was 99.26% and in the injections, 102.08%. The optimized and validated method may be successfully employed to perform routine quality control analyses.

Analysis of organic impurities of besifloxacin hydrochloride by high performance liquid chromatography with isocratic and gradient elution.

2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Pharmaceutical Product ◽  
Raw Material ◽  
Isocratic Elution ◽  
Organic Impurities ◽  
Elution Method

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.

4-Nitrophenol in 4-nitrophenyl phosphate, a substrate for alkaline phosphatase, as measured by paired-ion high-performance liquid chromatography.

1977 ◽  
Vol 23 (12) ◽  
pp. 2288-2291 ◽  
Author(s):  
P H Culbreth ◽  
I W Duncan ◽  
C A Burtis
Keyword(s):  
Alkaline Phosphatase ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Nitrophenyl Phosphate ◽  
Phase Column ◽  
Reversed Phase Column

Abstract We used paired-ion high-performance liquid chromatography to determine the 4-nitrophenol content of 4-nitrophenyl phosphate, a substrate for alkaline phosphatase analysis. This was done on a reversed-phase column with a mobile phase of methanol/water, 45/55 by vol, containing 3 ml of tetrabutylammonium phosphate reagent per 200 ml of solvent. At a flow rate of 1 ml/min, 4-nitrophenol was eluted at 9 min and monitored at 404 nm; 4-nitrophenyl phosphate was eluted at 5 min and could be monitored at 311 nm. Samples of 4-nitrophenyl phosphate obtained from several sources contained 0.3 to 7.8 mole of 4-nitrophenol per mole of 4-nitrophenyl phosphate.

FORCED DEGRADATION STUDY OF ELETRIPTAN BY USING ULTRA HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (UHPLC)

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (07) ◽  
pp. 14-21
Author(s):  
S. Sahu ◽  
◽  
R.M Singh ◽  
S.C. Mathur ◽  
D. K Sharma ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Degradation Study ◽  
Liquid Chromatography Method ◽  
Isocratic Mode

A simple, fast, precise and accurate ultra high performance liquid chromatography method was developed for degradation study of eletriptan hydrobromide (EH) under exaggerated conditions. An Inertsil ODS C18 (250 x 4.6 mm, 5µm) column in isocratic mode was used with mobile phase comprising of water, methanol and trifluoroacetic acid mixed in the ratio 55:45:0.1 % V/V/V, maintained at pH 3.5. The flow rate was set at 0.4 mL per minute with UV detection at 225 nm. The retention time of EH was found to be 3.7 minutes. Linearity for EH was found in the range of 3.5- 200 µg per mL and percentage recoveries were obtained in the range of 100.2 % to 100.6 %. The method was capable of resolving all degradants and principle component in sample. The proposed method is accurate, precise, selective, reproducible, and rapid for detection of degradation of eletriptan hydrobromide.

scholarly journals DEVELOPMENT OF A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR ANALYZING DISODIUM 5′-GUANYLATE AND DISODIUM 5′-INOSINATE LEVELS IN FLAVOR ENHANCERS

2018 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Dwi Karina Natalia ◽  
Harmita . ◽  
Taufiq Indra Rukmana
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Array Detector ◽  
Potassium Phosphate Buffer ◽  
Chromatography Method

Objective: This study aimed to develop a selective analytical method for assessing disodium 5′-guanylate and disodium 5′-inosinate levels in flavorenhancers.Methods: The levels were assessed using high-performance liquid chromatography (HPLC) with a photodiode array detector (PDA) (wavelength=255 nm) and a SunFire® C18 column (250 mm × 4.6 mm × 5 μm). The mobile phase comprised a mixture of potassium phosphate buffer and anion pair reagent-hexane-1-sulfonic acid sodium salt - with a flow rate of 1.2 mL/min. The ion pair was used to generate a neutral equilibrium, whichresulted in increased retention of the analytes. Optimized analysis conditions were then validated regarding accuracy, precision, linearity, selectivity,and the limits of detection and quantification.Results: The average levels of disodium 5′-inosinate in the six analyzed samples were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and0.47±2.21%, respectively. Regarding disodium 5′-guanylate, the average levels were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and0.34±1.83, respectively.Conclusion: The optimal conditions for analyzing disodium 5′-guanylate and disodium 5′-inosinateusing HPLC with a PDA and SunFire C18 columnwere λ=255 nm, a mobile phase of potassium phosphate buffer and sodium hexane sulfonate, and a flow rate of 1.2 mL/min. For disodium 5′-inosinate,its average levels in samples A–F were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and 0.47±2.21%, respectively. Meanwhile, the averagelevels of disodium 5′-guanylate in the samples were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and 0.34±1.83%, respectively.

scholarly journals Reverse-phase High-Performance Liquid Chromatography Method Development and Validation for Estimation of Glimepiride in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 296-302
Author(s):  
Aseem Kumar ◽  
Anil Kumar Sharma ◽  
Rohit Dutt
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

The present work demonstrates a simple, rapid, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method for analyzing glimepiride in pure and tablet forms. The present method was developed using a C18 column 150 × 4.6 mm, with 5 μm, and packing L1 maintained at a temperature of 30°C. The mobile phase was prepared by dissolving 0.5 gram of monobasic sodium phosphate in 500 mL of distilled water, pH of the solution adjusted to 2.1 to 2.7 with 10% phosphoric acid, and added 500 mL of acetonitrile. The mobile phase was pumped in the highperformance liquid chromatography (HPLC) system at a flow rate of 1 mL/min, and separation was carried out at 228 nm, using an ultraviolet (UV) detector. The chromatographic separation was achieved with peak retention time (RT) at about 9.30 minutes, and the method was found to be linear over a concentration range of 40 to 140 μg/mL. The specificity of the method represented no interference of the excipients during the analysis, and stability testing after 24 hours also showed that the method is suitable and specific. The accuracy was between 99.93 to 99.96%, with limit of detection (LOD) and limit of quantitation (LOQ) being 0.354 μg/mL, 1.18 μg/mL, respectively. Satisfactory results were found for precision and robustness parameters during the development and validation stage for the analytical method. The proposed method was also adopted for the analysis of glimepiride tablets to improve the overall quality control. Using this method, symmetric peak shape was obtained with reasonable retention time. The retention time of glimepiride for six repetitions is 9.3 ± 0.1 minutes; the run time is 21 minutes. The proposed RP-HPLC method is a modification of the United States Pharmacopeia (USP) method, and it was found to be valid for glimepiride within concentration ranges 40 to 140 μg/mL, using C18 analytical columns, and isocratic elution with UV detection, and at 1 mL/min of flow rate.

Simple Continuous and Simultaneous Determination of Multiple Sulfonamide Residues

1993 ◽  
Vol 56 (12) ◽  
pp. 1067-1072 ◽  
Author(s):  
CHIN-EN TSAI ◽  
FUSAO KONDO
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Correlation Coefficients ◽  
Inhibition Zone ◽  
Agar Block ◽  
Minimum Medium

A new continuous separation method was developed for the determination of nine different sulfonamides (sulfaguanidine, sulfamethazine, sulfapyridine, sulfadiazine, sulfathiazole, sulfamethizole, sulfamethoxazole, sulfadimethoxine, and sulfaquinoxaline). Bioassay on minimum medium seeded with Bacillus subtilis ATCC 6633 was carried out for detection. An extract taken from an agar block of the clear inhibition zone on minimum medium produced by a mixture of sulfonamides was then subjected to high-performance liquid chromatography. For identification, high-performance liquid chromatography analyses were performed using two different columns and analytical conditions. Using a μ-Bondapak C18 column, the sulfonamides were separated at room temperature using a mobile phase of methanol: 0.1 M KH2PO4 (30:70, vol/vol) at a flow rate of 1.0 ml/min. A variable wavelength detector set at 265 nm and recorder set at 4 mm/min were used for the detection. The entire mixture was resolved as eight peaks from 4.68 to 50.78 min. When an Asahipak GS-320 column was employed, nine peaks were separated with retention times ranging from 12.62 to 54.43 min using a mobile phase of acetonitrile: 1% acetic acid (25:75, vol/vol) at a flow rate of 2.0 ml/min. Correlation coefficients of standard curves for individual sulfonamides were linear (&gt;0.99) with recoveries ranging from 25.2 ± 8.6% to 64.1 ± 8.6% for a concentration range of 1.0–25 μg/ml.

Development and validation of high-performance liquid chromatography method for the simultaneous monitoring of pantoprazole sodium sesquihydrate and domperidone maleate in plasma and its application to pharmacokinetic study

2020 ◽  
Vol 32 (3) ◽  
pp. 157-165
Author(s):  
Ghulam Abbas ◽  
Malik Saadullah ◽  
Akhtar Rasul ◽  
Shahid Shah ◽  
Sajid Mehmood Khan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phase Composition ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Mobile Phase Composition ◽  
Chromatography Method ◽  
Surface Design

A sensitive, inexpensive high-performance liquid chromatography–ultraviolet detection (HPLC–UV) method has been developed and validated for the simultaneous monitoring of pantoprazole sodium sesquihydrate (PSS) and domperidone maleate (DM) in rabbit plasma on a C18 column with UV detection at 285 nm. Box–Behnken design was used with 3 independent variables, namely, flow rate (X1), mobile phase composition (X2), and phosphate buffer pH (X3), which were used to design mathematical models. Response surface design was applied to optimize the dependent variables, i.e., retention time (Y1 and Y2) and percentage recoveries (Y3 and Y4) of PSS and DM. The method was sensitive and reproducible over 1.562 to 25 μg/mL. The effect of the quadratic outcome of flow rate, mobile phase composition, and buffer pH on retention time (p ˂ 0.001) and percentage recoveries of PSS and DM (p = 0.0016) were significant. The regression values obtained from analytical curve of PSS and DM were 0.999 and 0.9994, respectively. The percentage recoveries of PSS and DM were ranged from 94.5 to 100.41% and 94.77 to 100.31%, respectively. The developed method was applied for studying the pharmacokinetics of PSS and DM. The Cmax of test and reference formulations were 48.06 ± 0.347 μg/mL and 46.31 ± 0.398 μg/mL for PSS, and 15.11 ± 1.608 μg/mL and 12.06 ± 1.234 μg/mL for DM, respectively.

scholarly journals Determination of the Analgesic Components of Spasmomigraine® Tablet by Liquid Chromatography with Ultraviolet Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 94-101 ◽  
Author(s):  
Fawzy A Elbarbry ◽  
Mokhtar M Mabrouk ◽  
Mohamed A El-Dawy
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ambient Temperature ◽  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
Dosage Forms ◽  
Ultraviolet Detection

Abstract A procedure was developed for the determination of the analgesic components of Spasmomigraine® tablets, which are ergotamine (I), propyphenazone (II), caffeine (III), camylofin (IV), and mecloxamine (V). They were subjected to high-performance liquid chromatography on a column (300 × 3.9 mm, 10 μm particle size) packed with μ-Bondapak C18. Separations were achieved with the mobile phase methanol–water–triethylamine (60 + 40 + 0.1, v/v/v) flowing at a rate of 1.5 mL/min, and quantitative determination was performed at 254 nm at ambient temperature for I–III; acetonitrile–25 mM KH2PO4–acetic acid (45 + 55 + 0.2, v/v/v), flowing at a rate of 1.5 mL/min and detection at 234 nm at ambient temperature, was used for IV and V. Methyl paraben was used as an internal standard. The detection limits were 0.35 (I), 5.0 (II), 1.5 (III), 3.0 (IV), and 2.0 g/mL (V). The method was accurate (mean recovery 98 ± 2%, n = 4) and precise (coefficient of variation &lt;5%, n = 5). The proposed method is rapid and sensitive and, therefore, suitable for the routine control of these ingredients in multicomponent dosage forms.

scholarly journals RP-LC and TLC Densitometric Determination of Paracetamol and Pamabrom in Presence of Hazardous Impurity of Paracetamol and Application to Pharmaceuticals

2013 ◽  
Vol 8 ◽  
pp. ACI.S12349 ◽  
Author(s):  
Ola Mohamed El-Houssini
Keyword(s):  
High Performance Liquid Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Thin Layer ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Column Temperature ◽  
Layer Chromatography

Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100-600 and 4-24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1-10 and 0.32-3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets.

Sign in / Sign up

Export Citation Format

Share Document