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.

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.

scholarly journals Determination of rutin content in sophora japonia L. Extracts used as raw material in supplements by high performance liquid chromatography

2019 ◽  
Vol 2 (3) ◽  
pp. 51-55
Author(s):  
Dat Nguyen Thanh ◽  
Hong Hanh Nguyen Thi ◽  
Thu Dam Thi ◽  
Thuy Chu Thi ◽  
Nuong Hoang Thi ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Acid Solution ◽  
Mobile Phase ◽  
High Performance ◽  
Acetic Acid Solution ◽  
Raw Material ◽  
Sophora Japonica

An HPLC-UV method was proposed in order to determine Rutin in Sophora japonica L. extract samples (3 samples extracted with 30% ethanol, 3 samples extracted with 70% ethanol and 3 samples extracted with water). The chromatographic conditions were: Agilent Zorbax Eclipse XDB C18 Column (150 x 4.6 mm, 5 µm); UV-Vis detector (257 nm); mobile phase: a mixture of methanol and 1% acetic acid solution (40:60, v/v). The linear range was of 4.97 - 298.47µg/mL; the LOQ was of 0.205 µg/mL and the accuracy was within 99.87% - 102.3%. The method was proved to be suitable for the determination of Rutin in Sophora japonica L. extracts. Rutin content in samples varied from 30.14% to 38.67%.

scholarly journals Determination of protodioscin in tribulus terrestris by reversed-phase high-performance liquid chromatography

2021 ◽  
Vol 284 ◽  
pp. 03002
Author(s):  
Mikhail Sergeev ◽  
Georgiy Zaitsev ◽  
Dmitry Yermolin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Raw Materials ◽  
Reversed Phase ◽  
Phosphoric Acid Solution ◽  
Biologically Active ◽  
Raw Material ◽  
Tribulus Terrestris ◽  
Column Temperature

In this study, high performance liquid chromatography (HPLC) was used to analyze the protodioscin content in Tribulus terrestris samples. They were separated by C18 chromatography column, gradient with 0.1 % phosphoric acid solution and acetonitrile was used as the mobile phase with the flow rate of 0.5 mL/min, the column temperature was 45 °C, and the detection wavelength was 203 nm. The results showed that the protodioscin content has a good linear correlation (r>0.999) within the range of 50 mg/L to 1500 mg/L. In samples of raw material from Crimea it was found: 0.546 % ± 0.013 protodioscin and in analyzed material from Western Siberia it was 0.338% ± 0.008 for n=3. Raw materials of Tribulus terrestris growing in Crimea are more promising than similar raw materials from the West Siberian region due to the higher content of protodioscin for the production of biologically active products containing steroid saponins.

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.

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