scholarly journals Bioanalytical method validation of Esomeprazole by high performance liquid chromatography with PDA detection

2020 ◽  
Author(s):  
Fatema Moni ◽  
Suriya Sharmin ◽  
Satyajit Roy Rony ◽  
Farhana Afroz ◽  
Shammi Akhter ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Precipitation Method ◽  
Dihydrogen Phosphate ◽  
Serum Samples ◽  
Bioanalytical Method Validation ◽  
Relative Standard

AbstractThis study describes the development and validation of a simple, specific, accurate, and precise method for quantitative determination of Esomeprazole in human serum using Pantoprazole as internal standard (IS). After the addition of internal standard, Esomeprazole from serum samples was extracted simply by protein precipitation method followed by centrifugation and the supernatants were directly injected into the high performance liquid chromatography (HPLC). The chromatographic separation of the compounds was obtained on Hitachi Lachrom C8 column (5 µm, 250 × 4.6 mm) with a mobile phase consisting of 5 mM potassium dihydrogen phosphate pH 7.4 and acetonitrile in a ratio of 70:30 with UV detection at 302 nm with a flow rate of 1 mL/min. The method was sensitive and specific, and validated over a concentration range of 0.06–6.0 µg/mL. The limit of detection (LOD) and lower limit of quantification (LOQ) was 0.03 µg/mL and 0.06 µg/mL, respectively. The precision and accuracy expressed as relative standard deviation were less than 15%. The average recovery of Esomeprazole from serum was 97.08%.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF DEOXYARBUTININ ANHYDROUS EMULSION SYSTEM USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 172-175 ◽  
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Emulsion System ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

scholarly journals STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION OF METFORMIN AND ERTUGLIFLOZIN BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY WITH PDA DETECTION AND ITS APPLICATION TO TABLET DOSAGE FORM

2019 ◽  
pp. 353-358
Author(s):  
KADALI JAGADEESH ◽  
ANNAPURNA N
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Phase System ◽  
Dihydrogen Phosphate ◽  
Response Measurement ◽  
Stability Indicating ◽  
Relative Standard

Objective: A sensitive, rapid, accurate, and precise stability indicating high-performance liquid chromatography method was developed and validated for the simultaneous estimation of metformin (MET) and ertugliflozin (ERT). Methods: The planned chromatographic method was developed using Kromasil C18 column using 0.1 M sodium dihydrogen phosphate methanol (50:50, by volume, pH 4.0) as mobile phase system followed by peak area response measurement at 238 nm. The developed method was validated by means of ICH guidelines about system suitability, linearity, sensitivity, selectivity, accuracy, precision, robustness, and specificity. Results: Calibration curves of MET and ERT are linear from 250 to 750 μg/ml and 3.75 to 11.25 μg/ml, respectively. Relative standard deviation is <2.0% and recovery is ̴ 100%. Successfully, the developed method was applied for the simultaneous determination of MET and ERT in tablets and to study degradation of MET and ERT in acidic, alkaline, oxidation, thermal, and photolytic degradation conditions. No obstructions from additional common excipients of tablets and degradants were observed. Conclusion: The results recommended method suitability for the analysis of MET and ERT in quality control laboratories.

scholarly journals Microextraction by Packed Molecularly Imprinted Polymer Combined Ultra-High-Performance Liquid Chromatography for the Determination of Levofloxacin in Human Plasma

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Jia Meng ◽  
Xu Wang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Bacterial Infections ◽  
High Performance ◽  
Limit Of Detection ◽  
Binding Capacity ◽  
Molecularly Imprinted ◽  
Relative Standard

Fluoroquinolones are considered as gold standard for the prevention of bacterial infections. To improve assessment of antibacterial efficacy, a novel method for determination of levofloxacin was developed and validated. Deep eutectic solvents (DESs) as only green solvent were used as a porogen for preparation of water-compatible molecularly imprinted polymers (MIPs) with a pseudotemplate. The DESs-MIPs were characterized in detail, including scanning electron microscope, nitrogen sorption porosimetry, and Fourier transform-infrared spectra. Clearly, the maximum binding capacity of levofloxacin on DESs-MIPs in water and methanol was 0.216 and 0.077 μmol g−1, respectively. The DESs-MIPs as adsorbing materials were applied in microextraction by packed sorbent (MEPS), and the DESs-MIPs-MEPS conditions were optimized. The DESs-MIPs-MEPS coupled with ultra-high-performance liquid chromatography (UHPLC) was used to determine levofloxacin in human plasma. The method was found linear over 0.05–10 μg mL−1 with coefficient of correlation equal to 0.9988. The limit of detection and limit of quantification were 0.012 and 0.04 μg mL−1, respectively. At three spiked levels, the precision of proposed method was between 95.3% and 99.7% with intraday and interday relative standard deviations ≤8.9%. Finally, the developed method was used to examine levofloxacin from human plasma of 20 hospitalized patients after transrectal ultrasound-guided prostate biopsy, and the average concentration (±SD) of levofloxacin was 2.35 ± 0.99 μg mL−1 in plasma.

scholarly journals Determination of Imazaquin Residues in Soil by Solid-Phase Extraction and High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (2) ◽  
pp. 568-574 ◽  
Author(s):  
Chen Xuyan ◽  
Hu Jiye ◽  
Li Jianzhong
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Application Rates ◽  
Relative Standard ◽  
Strong Anion Exchange

Abstract A method has been developed for the quantitation of imazaquin residues in soil. The herbicide was extracted from soil with methanolwater (2 + 1, v/v) and cleaned up by strong anion-exchange solid-phase extraction cartridges. Analysis was performed by using high-performance liquid chromatography with ultraviolet detection. Average recoveries through the method ranged from 90.7 to 100.6%, with relative standard deviation equal to or lower than 6.6%. The limit of detection was estimated to be 0.0015 mg/kg, and the minimum quantitation concentration of imazaquin in soil was 0.005 mg/kg. This method was successfully applied to evaluate imazaquin residue levels in soil and its dissipation rates in a soybean field in the Xisanqi District of Beijing, People's Republic of China. The dissipation study showed that the half life of imazaquin in soil was 10.37 0.0135 days at 3 different application rates.

scholarly journals Development, Validation, and Routine Application of a High-Performance Liquid Chromatography Method Coupled with a Single Mass Detector for Quantification of Itraconazole, Voriconazole, and Posaconazole in Human Plasma

2010 ◽  
Vol 54 (8) ◽  
pp. 3408-3413 ◽  
Author(s):  
Lorena Baietto ◽  
Antonio D'Avolio ◽  
Giusi Ventimiglia ◽  
Francesco Giuseppe De Rosa ◽  
Marco Siccardi ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Internal Standard ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
True Value ◽  
Relative Standard ◽  
Mass Detector ◽  
Liquid Chromatography Method

ABSTRACT We have developed and validated a high-performance liquid chromatography method coupled with a mass detector to quantify itraconazole, voriconazole, and posaconazole using quinoxaline as the internal standard. The method involves protein precipitation with acetonitrile. Mean accuracy (percent deviation from the true value) and precision (relative standard deviation percentage) were less than 15%. Mean recovery was more than 80% for all drugs quantified. The lower limit of quantification was 0.031 μg/ml for itraconazole and posaconazole and 0.039 μg/ml for voriconazole. The calibration range tested was from 0.031 to 8 μg/ml for itraconazole and posaconazole and from 0.039 to 10 μg/ml for voriconazole.

scholarly journals Estimation of Atenolol by Reverse Phase High Performance Liquid Chromatography

2010 ◽  
Vol 7 (3) ◽  
pp. 962-966 ◽  
Author(s):  
Naveen Kumar ◽  
Nishant Verma ◽  
Omveer Songh ◽  
Naveen Joshi ◽  
Kanwar Gaurav Singh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Equal Proportion ◽  
Uv Detector ◽  
Chromatography Method ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Method

A simple, precise, sensitive, fast and accurate high performance liquid chromatography method has been developed for the determination of atenolol using mixture of phosphate buffer and acetonitrile (53:47 v/v) as mobile phase. Buffer was prepared by mixing 0.02 M K2PO4and 0.003 M KH2PO4in equal proportion. Detection was carried out using UV detector at λmax230 nm. Column was ODS and dimensions of column was 25 mm × 4.6 mm. Atenolol was eluted out at retention time of 2.1 min. Method was validated at 1.2 mL/min flow rate. Calibration curve was linear between ranges of 40 to 200 mcg concentration. The limit of detection was calculates 120 nano gram and limit of quantitation is 510 nano gram. The relative standard deviation (RSD) of atenolol was 0.6. The percentage recovery of atenolol was 99.6%.

scholarly journals Extraction and Determination of Oxymatrine Pesticide in Environmental Sample and in its Formulation using High-Performance Liquid Chromatography

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.

scholarly journals Determination of the total tryptophan in food by high performance liquid chromatography combined with enzyme hydrolysis

2019 ◽  
Vol 2 (2) ◽  
pp. 37-43
Author(s):  
Huyen Trang Luu Thi ◽  
Trang Vu Thi ◽  
Ngan Le Viet ◽  
◽  
◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Standard Addition ◽  
Reversed Phase ◽  
Enzyme Hydrolysis ◽  
Protease Enzyme

High performance liquid chromatography was applied for the determination of tryptophan in&nbsp;food. The sample was hydrolyzed in a duration from 16 to 24 hour by protease enzyme at 50 oC.&nbsp;The extract was separated on the C8 reversed phase column with mobile phase of NaH2PO4 50mM&nbsp;pH 2.3: Methanol (82:18; v/v). The linearity of the method was kept in the range of 0.5 - 50 mg/L.&nbsp;Limit of detection was found to be 4.6 mg/100g. Recovery was determined by standard addition&nbsp;method, giving values of recovery in the range of 97 - 103% and RSD (n = 6) in the range of 0.077 -&nbsp;2.27%. Internal standard was used to reduce the errors in analysis process and good reproducibility.

scholarly journals Analysis of Ethyl p-Methoxycinnamate from Kaempferia galanga L. Extract by High Performance Liquid Chromatography

2021 ◽  
Vol 5 (4) ◽  
pp. 353-358
Author(s):  
Wiwin Winingsih ◽  
Sri Gustini Husein ◽  
Rozalia Putri Neno Ramdhani
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Range Limit ◽  
Uv Detector ◽  
Kaempferia Galanga ◽  
System Suitability ◽  
Relative Standard ◽  
Limit Of Quantitation

Ethyl para-methoxycinamate (EPMS) is a major compound of Kaempferia galanga L that has anti-inflammatory effect.  The purpose of this study was to determine of EPMS in Kaempferiae galanga L rhizome extract by  High Performance Liquid Chromatography (HPLC) and evaluated the performance of the analysis. This study included determination of system suitability, accuracy, precision, linearity and range, limit of detection (LOD) and Limit of quantitation (LOQ) and selectivity.  The results of system suitability test  HPLC System for EPMS analysis were as follows isocratic elution system of a mobile phase mixture of methanol: water (70:30) containing 0.1% TFA, uv detector at a wavelength of 308 nm using column C18 (150 × 4, 6mm, 5μm) flow rate 1 ml / min. From the analysis, it was found that the average EPMS content was 78.74%. Then method had linear concentration range from 5-360 ppm, with R ² = 0.9999. The LOD and LOQ were 7.0722 ppm and 21.4311 ppm respectively. The accuracy of this method that represented by % recovery was 98.02% - 101.26%. The precision of this method that expressed by Relative Standard Deviation (RSD) was 1.57%. The selectivity of this method that showed by  resolution value was 2.6. Based on the results of the system suitability test and analysis performance evaluation,all parameters met the requirements.

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