scholarly journals Determination of Ketotifen Fumarate in Syrup Dosage Form by High Performance Liquid Chromatography

Author(s):  
Mohammed Ali Salih ◽  
Dlivan Fattah Aziz ◽  
Salar Ibrahim Ali

The goal of the current study was to establish and authenticate an isocratic reverse-stage High-Performance Liquid Chromatography (HPLC) method for quantifying ketotifen fumarate (KF) in pharmaceutical liquid dosage compositions. Easy, quick, accurate, exact, and accurate reverse-stage high-performance liquid chromatography was advanced for the simultaneous assessment of ketotifen fumarate in the liquid syrup dosage type. The HPLC system using isocratic elution method with reverse-phase Inertsil ODS-(250 mm × 4.6 mm, 3 μm) column was detected by ultraviolet absorbance at 297 nm with no interference from widely using excipients, the mobile phase (A) is a mixture of triethylamine and water (175 μl in 500 ml of water), and the mobile phase (B) is a mixture of triethylamine and methanol (175 μl in 500 ml of methanol) at a flow rate of 1.5 mL/min (mobile phase A 40 %:mobile phase B 60%) at column temperature using 40 ° C, the retention time for ketotifen fumarate was 6.4±0.5 min. The concentration curves were linear in the range of 10.0 to 35.0 μg / ml (R2 = 0.9999). The developed method was tested for the specificity, precision, linearity, precision, reliability, robustness, and consistency of the solution. The regeneration of ketotifen fumarate in formulations was found to be 99.75 %, 99.91 %, and 100.05 % respectively. The percent RSD for percent recovery was found to be 0.21 and 0.17 and 0.10 for ketotifen fumarate. In the conclusion, the suggested technique was successfully used for the quantitative determination of ketotifen fumarate in formulations.

2014 ◽  
Vol 998-999 ◽  
pp. 372-377 ◽  
Author(s):  
Qiang Wu ◽  
Chang Hong Wang ◽  
Pu Wang ◽  
Xiang Rong Liu

To examine the extraction method and chromatographic conditions that affect the determination of cinnamaldehyde in Baoyuanqingxue granules and make clinical evaluation about the determination of cinnamaldehyde.Ultrasonic methanol extraction was used before the detemination of cinnamaldehyde in Baoyuanqingxue granules. High Performance Liquid chromatography (HPLC) method was applied to detect samples. The SB-C18 column (Agilent, ZORBAX, 4.6×150mm, 5μm) was adopted, the mobile phase was acetonitrile-water (35:65) at the flow rate of 1.00mL•min-1 with DAD detection wavelength at 290nm, the volume of injection was 20μL and the column temperature was 30°C. The resolution between cinnamaldehyde and other peaks was good. The calibration curve was linear in the range of 0.5035~50.35μg•mL-1(r=0.99976). The average recovery (n=6) of cinnamaldehyde was 99.2% with RSD of 0.5%. The HPLC-DAD method to detect the content of cinnamaldehyde in Baoyuanqingxue granules is simple and accurate. It can be used for quality control of cinnamaldehyde in Baoyuanqingxue granules.


2012 ◽  
Vol 95 (4) ◽  
pp. 1064-1068 ◽  
Author(s):  
Mohammed H Mehanna ◽  
Abdel M Motawaa ◽  
Magda W Samaha

Abstract A reliable and sensitive HPLC method was developed for the quantitation of tadalafil transdermal permeation through human skin. An RP column with UV detection at 290 nm was used for chromatographic separation at ambient temperature. The mobile phase was acetonitrile–water containing 20 mM pH 7 phosphate buffer (35/65, v/v) with a flow rate of 1.0 mL/min. The LOQ achieved was 1 ng/mL, and the calibration curve showed good linearity over the concentration range of 5–2000 ng/mL for tadalafil, with a determination coefficient (R2) of 0.998. The RSD values of intraday and interday analyses were all within 7%. Parameters of validation proved the precision of the method; this validated method was applied for the determination of tadalafil in transdermal permeation and drug deposition in human skin studies.


2014 ◽  
Vol 675-677 ◽  
pp. 275-279 ◽  
Author(s):  
Su Su Fan ◽  
Jian Shi ◽  
Ling Zhou ◽  
Yu Wen Hang

Using the high performance liquid chromatography (HPLC) method, bifenthrin isomers can be split at a polysaccharide derivatives chiral stationary phase column, and two well distinguished peaks of bifenthrin isomers are obtained. The effects of mobile phase ratios, temperatures, and detection wavelengths on the separation results are discussed. The optimal chromatographic conditions are as follows: the mobile phase ratio is methanol: ammonium acetate salts = 80:20, the column temperature is 35°C, and the wavelength is set as 220 nm. Under the optimal conditions, the resolution of bifenthrin enantiomer can be as large as 3.0.


2020 ◽  
Vol 17 ◽  
Author(s):  
Lei Zheng ◽  
Jing Yang ◽  
Yu-yao Guan ◽  
Lei Zhang ◽  
Chao Song ◽  
...  

Background:: Establishing R, S-enantiomer (S-KT and R-KT) chiral resolution and determination methods for KT are of great significance. Objective:: This study aimed to establish a high-performance liquid chromatography (HPLC) method for the resolution and determination of ketorolac tromethamine (KT) enantiomers. Methods:: A CHIRALPAK AGP column (0.4  10 cm, 5 μm) was used with 10 mmol/L ammonium acetate (pH 5.5) and isopropanol (97:3) as the mobile phase. The detection wavelength was 324 nm, the flow rate was 1.0 mL/min, the column temperature was 25°C, and the injection volume was 5 μL. Results:: The resolution between S-KT and R-KT was 2.8. S-KT and R-KT demonstrated a good linear relationship in the range of 3-60 μg/mL (r > 0.999). The average recoveries of S-KT and R-KT were 99.2% and 99.8%, with relative standard deviations of 2.0% and 2.4%, respectively. Conclusion:: The established method can be used for the resolution and determination of S-KT and R-KT.


2013 ◽  
Vol 8 ◽  
pp. ACI.S12349 ◽  
Author(s):  
Ola Mohamed El-Houssini

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.


2017 ◽  
Vol 4 (1) ◽  
pp. 32-42 ◽  
Author(s):  
Assefa Takele ◽  
Abdel-Maaboud I. Mohamed Attaya ◽  
Ariaya Hymete ◽  
Melisew Tadele Alula

Introduction: Bromazepam is hydrolyzed in acidic aqueous solution leading to a series of degradation products. The rate of acidic hydrolysis is believed to be dependent on the state of protonation of the pyridyl and azomethine nitrogen atoms. Stability test is important in pharmaceutical industry to provide evidence on how the quality of an active substance or pharmaceutical product varies with time under the influence of a variety of environmental factors. Objective: The aim of the study was to develop a simple stability indicating method for the determination of bromazepam. Method: Bromazepam solution was prepared and forced degradation of bromazepam was performed under acid hydrolysis using sulphuric acid. High performance liquid chromatography determination of pure and degraded bromazepam and bromazepam-copper (II) complex was performed using reversed phase octyl C-8 column under isocratic conditions and the chromatographic conditions were set as follows; the flow rate of the mobile phase was 1.5 mL/min; injection volume was 10 μL, column temperature was 30oC and the detector wavelength being 309 nm. Results: Bromazepam, its degradation product and bromazepam chelated with copper (II) were determined using the developed mobile phase with flow rate of 1.5 mL/min. Good separation with sharp peak, minimum tailing and retention time repeatability was obtained. The rate order, rate constant and half-life of degradation were also determined, and it was observed that the degradation reaction follows the first order kinetics. Conclusion: Chromatographic separation of bromazepam chelated with copper (II) was achieved and the method can be further used in drug manufacturing quality control.


Author(s):  
Panchumarthy Ravisankar ◽  
Devala Rao G ◽  
Md Shaheem Sulthana ◽  
Supriya K ◽  
Mounika G ◽  
...  

Objective: Objective of the present investigation is to develop a speedy isocratic reverse phase high-performance liquid chromatography (RP-HPLC) method for the separation and quantitative determination of 5 angiotensin II - receptor antagonists, namely, telmisartan, losartan, valsartan, olmesartan, irbesartan, and atenolol along with thiazide diuretics mostly hydrochlorothiazide (HCTZ).Methods: RP-HPLC method was evolved using Welchrom C18 column (4.6 × 250 mm, 5 μm) as a stationary phase with the mobile phase comprising a variety of phosphate buffer with pH-3.3 and acetonitrile in the proportion of 50:50 v/v. The mobile phase was pumped at a current rate of 1 mL/minute. The detection wavelength was carried out at 230 nm.Results: The total run time was 6 minutes and the elution window of only 3 minutes. The peaks were eluted with decorous resolution. The calibration curves were linear (r2=0.9998) in all cases. The percentage relative standard deviation (RSD%) was <2% and average recovery was above 99.95%. The method was validated specificity, precision, and accuracy. High recovery values and low RSD% prove that this method is very accurate and reproducible. The developed method was applied to the estimation of the above-said drugs in binary combinations from different manufacturers which were a good agreement with label claim.Conclusion: The important advantage of developed method was that the five individual drugs can be determined on a single chromatographic system without alteration in detection wavelength and mobile phase composition. This novel method was statistically validated as per ICH guidelines. The optimized method proved to be linear, accurate, and robust. Hence, the above said proposed method was found to be a rapid tool for the routine determination of the above-said drugs in alone or combination with HCTZ in quality control analysis without interference of excipients.


2021 ◽  
Vol 233 ◽  
pp. 01023
Author(s):  
Yue Qiu ◽  
Qing Zhang ◽  
Genrong Li ◽  
Yingkun Gong ◽  
Mei Long

A high performance liquid chromatography (HPLC) method was established for the determination of two acrylate substances in environmental water. The optimal chromatographic conditions were determined via exploring the effects of chromatographic column, mobile phase, column temperature, flow rate, detection wavelength and other factors on the separation effect of acrylate substances. Finally, the effective separation of methyl methacrylate and isopropyl methacrylate was realized within 6 min. The retention time of the target compound was used for qualitative analysis and the external standard method was used for quantitative analysis in the experiment. The linear relationship between the two acrylates was good in the range of 0.2-50.0 mg/L, and the correlation coefficient of standard curve was higher than 0.999. The recovery rate was 88.6%-105.3%, the relative standard deviation was 1.7%-4.1%, and the detection limit (LODs) was 0.03-0.05 mg/L. The method was simple, efficient and accurate, and suitable for the determination of acrylates in environmental water samples.


2021 ◽  
Vol 33 (4) ◽  
pp. 930-936
Author(s):  
Khaldun M. Al Azzam ◽  
Ahmad Makahleh ◽  
Bahruddin Saad

A new simple and sensitive high-performance liquid chromatography (HPLC) method for the determination of formaldehyde in flour samples has been developed. Formaldehyde was quantified after derivatization with a readily available reagent, 2,4,6-trichlorophenyl hydrazine (TCPH) under basic conditions. The formaldehyde-TCPH derivative was eluted with chromatographic mobile phase of 70:30 (v/v) acetonitrile:water at a flow rate of 1.0 mL min–1; wavelength, 222 nm; injection volume, 50 μL, using a C18 ODS Hypersil column (250 mm × 4.5 mm, 5 μm). The calibration curve was linear over the range of 0.001-10 μg mL-1 with R2 = 0.999. Recoveries at three different concentration levels (0.1, 1.0 and 5 μg mL-1) ranged from 92.0-101.7% with RSD less than of 2.2%. The limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 1.0 ng mL-1, respectively. The developed method was used for the determination of formaldehyde in various flour-based samples.


2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.


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