Combination of Column Temperature Gradient and Mobile Phase Flow Gradient in Microcolumn and Capillary Column High-Performance Liquid Chromatography

1997 ◽  
Vol 69 (13) ◽  
pp. 2589-2593 ◽  
Author(s):  
F. Houdiere ◽  
P. W. J. Fowler ◽  
N. M. Djordjevic
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Temperature Gradient ◽  
Mobile Phase ◽  
High Performance ◽  
Capillary Column ◽  
Phase Flow ◽  
Column Temperature ◽  
Flow Gradient

Analysis of Bifenthrin and its Enantiomer Using High Performance Liquid Chromatography

2014 ◽  
Vol 675-677 ◽  
pp. 275-279 ◽  
Author(s):  
Su Su Fan ◽  
Jian Shi ◽  
Ling Zhou ◽  
Yu Wen Hang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Column Temperature ◽  
Polysaccharide Derivatives ◽  
Separation Results

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.

scholarly journals Related Impurities High-performance Liquid Chromatography Method Development and Validation for drug combinations: Olmesartan Medoxomil, Chlorthalidone and Cilnidipine

2020 ◽  
pp. 1-10
Author(s):  
Pranavkumar Shah ◽  
Bhavin Dhadhuk
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Olmesartan Medoxomil ◽  
Drug Combinations ◽  
Column Temperature ◽  
Related Impurities ◽  
Limit Of Quantitation ◽  
Run Time

The liquid chromatography mass spectrometry (LC-MS) compatible, stability-indicating, specific, linear, accurate, sensitive with less run-time related impurities reversed phase high-performance liquid chromatography (RP-HPLC) related impurities method has been developed for olmesartan medoxomil (OLM), chlorthalidone (CHLR), and cilnidipine (CIL) drug combinations, and the method has been validated according to ICH and US-FDA guidelines. The chromatographic separation was performed by using Hypersil-BDS Thermo-Scientific, C18 (12.5 cm, 4.6 mm, 5 microns particle size) column. Mobile phase-A was prepared by mixing 3.85 gm ammonium acetate in HPLC water and adjust pH 5.0 by using diluted acetic acid. Acetonitrile was taken as mobile phase-B. Initial mobile phase ratio (55:45 v/v) was adjusted for mobile phase-A: mobile phase-B followed by gradient program. Other chromatographic conditions such as column temperature 25 degrees, flow rate 1.0 mL/minutes with the detection wavelength at 260 nm. The retention time for CHLR impurity A, olmesartan (OL), OLM impurity A, were found about 2.7, 3.3, and 7.2 minutes respectively, with a total run time of 18.0 minutes. The linearity calibration plot was performed and found linear relationship over the concentration range of 1.25 limit of quantitation (LoQ)–18.75 μg/mL, 3.6 LoQ–60.0 μg/mL, 3.6 LoQ–60.0 μg/mL respectively for CHLR impurity A, OL and OLM impurity A respectively. The limit of detection (LoD) and LoQ were found 0.4 ppm (μg/mL) and 1.2 ppm (μg/mL), 1.2 ppm (μg/mL) and 3.5 ppm (μg/mL), 1.1 ppm (μg/mL) and 3.3 ppm (μg/mL) for CHLR impurity A, OL and OLM impurity A respectively. The accuracy was determined by recovery studies and was found between 90.0–110.0%. The developed analytical method has been validated for LoD-LoQ, specificity, linearity, accuracy, precision, robustness, and ruggedness, which were well within the acceptance limit as per ICH guidelines. All the degradation products generated by stress conditions were found to be well separated from one another (all drug components and impurities). The developed method with shorter runtime was successfully implemented for routine quality control and stability analysis to check the quality of OLM, CHLR, and CIL drug combinations.

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

2020 ◽  
pp. 63-72
Author(s):  
Mohammed Ali Salih ◽  
Dlivan Fattah Aziz ◽  
Salar Ibrahim Ali
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Ketotifen Fumarate ◽  
Suggested Technique ◽  
Elution Method

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.

scholarly journals Direct Enantiomeric Separation and Determination of Hexythiazox Enantiomers in Environment and Vegetable by Reverse-Phase High-Performance Liquid Chromatography

2020 ◽  
Vol 17 (10) ◽  
pp. 3453
Author(s):  
Ping Zhang ◽  
Sheng Wang ◽  
Dongmei Shi ◽  
Yangyang Xu ◽  
Furong Yang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Enantiomeric Separation ◽  
Reverse Phase ◽  
Column Temperature ◽  
Resolution Factor ◽  
Phase Temperature ◽  
Lower Temperature

In the present study, the direct enantiomeric separation of hexythiazox enantiomers on Lux cellulose-1, Lux cellulose-2, Lux cellulose-3, Lux cellulose-4, Lux amylose-1 and Chirapak IC chiral columns were carefully investigated by reverse-phase high-performance liquid chromatography (RP-HPLC). Acetonitrile/water and methanol/water were used as mobile phase at a flow rate of 0.8 mL·min−1. The effects of chiral stationary phase, temperature, thermodynamic parameters, mobile phase component and mobile phase ratio on hexythiazox enantiomers separation were fully evaluated. Hexythiazox enantiomers received a baseline separation on the Lux cellulose-3 column with a maximum resolution of Rs = 2.09 (methanol/water) and Rs = 2.74 (acetonitrile/water), respectively. Partial separations were achieved on other five chiral columns. Furthermore, Lux amylose-1 and Chirapak IC had no separation ability for hexythiazox enantiomers when methanol/water was used as mobile phase. Temperature study indicated that the capacity factor (k) and resolution factor (Rs) decreased with column temperature increasing from 10 °C to 40 °C. The enthalpy (ΔH) and entropy (ΔS) involved in hexythiazox separation were also calculated and demonstrated the lower temperature contributed to better separation resolution. Moreover, the residue analytical method for hexythiazox enantiomers in the environment (soil and water) and vegetable (cucumber, cabbage and tomato) were also established with reliable accuracy and precision under reverse-phase HPLC condition. Such results provided a baseline separation method for hexythiazox enantiomers under reverse-phase conditions and contributed to an environmental and health risk assessment of hexythiazox at enantiomer level.

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.

Establishment and Evaluation of Determination of Cinnamaldehyde in Baoyuanqingxue Granules by HPLC

2014 ◽  
Vol 998-999 ◽  
pp. 372-377 ◽  
Author(s):  
Qiang Wu ◽  
Chang Hong Wang ◽  
Pu Wang ◽  
Xiang Rong Liu
Keyword(s):  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Extraction Method ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Average Recovery

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.

A Quality by Design (QbD) Based Method Development and Validation of a High-Performance Liquid Chromatography for the Simultaneous Estimation of Metformin and Ertugliflozin

2021 ◽  
Vol 12 (3) ◽  
pp. 1709-1717
Author(s):  
Haritha G ◽  
Vijey Aanandhi M ◽  
Shanmugasundaram P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Quality By Design ◽  
Simultaneous Estimation ◽  
Chromatography Method ◽  
Column Temperature ◽  
Relative Standard

This study explains about the Analytical Quality by Design approach for the optimization of a High-Performance Liquid Chromatography Method for the simultaneous estimation of Metformin and Ertugliflozin in pharmaceutical substance. The study aimed to optimize the High-Performance Liquid Chromatography (HPLC) by means of an analytical target profile in order to achieve good separation of compounds along with acceptable analysis time. Identification of risk factors for variables affects the method efficacy. This leads to the development of an accurate, precise, and economic method. The optimized conditions of the developed method were a stationary phase of a Discovery C18 250 x 4.6mm, 5m and a mobile phase of Orthophosphoric acid buffer (pH 2.2),ACN taken in the ratio 60:40 was selected as mobile phase and detection wavelength of 230nm. The flow rate was selected as 0.98ml/min at 29.150C column temperature. Using the central composite design (CCD) method was optimized. The method is showing the linearity over the concentration range of 25-150µg/ml for Metformin and 0.375-2.25µg/ml for Ertugliflozin. The intra-and inter-day precision were less than 2% of relative standard deviation. Accuracies between  99-102% of the true values.The LOD obtained for Metformin and Ertugliflozin were found to be 59 and 3.7, respectively.  LOQ obtained for Metformin and Ertugliflozin were 77.6 and 5.2, respectively.Under accelerated conditionsdegradation percentage of the drug was found to be less than 10%, and the degradation product peak not affecting the system suitability of Metformin and Ertugliflozin.

scholarly journals High Performance Liquid Chromatography (HPLC) Stability Indicating Method for the Determination of Bromazepam Via its Copper (II) Chelates

2017 ◽  
Vol 4 (1) ◽  
pp. 32-42 ◽  
Author(s):  
Assefa Takele ◽  
Abdel-Maaboud I. Mohamed Attaya ◽  
Ariaya Hymete ◽  
Melisew Tadele Alula
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Azomethine Nitrogen ◽  
Column Temperature ◽  
Stability Indicating ◽  
Stability Indicating Method

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.

scholarly journals Analysis of citric acid and D-isoascorbic acid in beverages by High performance liquid chromatography

2021 ◽  
Vol 251 ◽  
pp. 02047
Author(s):  
Rui Wang ◽  
Shiwen Hu ◽  
Jie Chen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Citric Acid ◽  
Acid Solution ◽  
Mobile Phase ◽  
High Performance ◽  
Phosphoric Acid Solution ◽  
Column Temperature ◽  
Isoascorbic Acid ◽  
Good Linear Correlation

In this study, high performance liquid chromatography (HPLC) was used to analysis the content of citric acid and D-isoascorbic acid in beverages. The samples were separated by C18 chromatography column, 0.1 % phosphoric acid solution was used as the mobile phase with the flow rate of 0.5 mL/min, the column temperature was 35 °C, and the detection wavelength was 210 nm. The results showed that the content of citric acid and D-isoascorbic acid has a good linear correlation (r>0.99) within the range of 50 μg to 200 μg. The selectivity, recovery and precision of citric acid and D-isoascorbic acid were suitable. Meanwhile, this method could be used to detect the content of citric acid and D-isoascorbic acid in beverages.

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