Beta-Alanine and Tris-(hydroxyl methyl) Aminomethane as Peak Modifiers in the Development of RP–HPLC Methods Using Aceclofenac and Haloperidol Hydrochloride as Exemplar Drugs

2021 ◽  
Author(s):  
Ramalingam Peraman ◽  
Pokuri Chiranjeevi ◽  
Yerrigamreddy Padmanabha Reddy ◽  
Kondreddy Vinod Kumar ◽  
S G Vasantharaju ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Analytical Approach ◽  
Water Solubility ◽  
Array Detector ◽  
Beta Alanine ◽  
Rp Hplc ◽  
Null Effect ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Theoretical Plates

Abstract In the present analytical approach, beta-alanine (ALA) and tris-(hydroxyl methyl) aminomethane (TRIS) were investigated as peak modifiers due to their water solubility and their possible peak modifying a property. These reagents were tested for their efficacy on the elution of aceclofenac (ACF) and haloperidol hydrochloride (HLC) from C18 column (250 mm × 4.6 mm, 5 μ) equipped with a photodiode array detector. The test reagents were investigated at 0.25 ± 0.05% concentration with a varying % aqueous composition on elution efficacy of HLC and ACF. The added ALA/TRIS in the mobile phase significantly (P < 0.05) improvised the symmetrical elution of HLC with 3-fold theoretical plates increase (P < 0.05) and 10-fold reduced capacity factor as compared to the control run. For ACF, the shoulder effect observed for ACF peak was eliminated. The optimized mobile phase was a combination of acetonitrile and water containing 0.25% beta-alanine/TRIS (pH 3.5 with ortho-phosphoric acid) at the ratio of 70:30 and 60:40% v/v, respectively, for ACF and HLC. The method was validated as per ICHQ2 guidelines. The column performance was tested for reproducibility in non-peak modifier applications and revealed a null effect on the column, thus these agents are relatively less toxic to HPLC columns.

STABILITY INDICATING ASSAY METHOD OF SIROLIMUS USING HPLC AND SEPARATION OF ACID DEGRADANT BY HPTLC

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (04) ◽  
pp. 48-55
Author(s):  
S. Jadhav ◽  
◽  
P. Pisal ◽  
M. Mahajan
Keyword(s):  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Oxidation Stress ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
The Given ◽  
Stressed Sample

A stability indicating RP-HPLC method has been developed and subsequently validated for Sirolimus. The proposed RP-HPLC method utilizes Phenomenex, C18, 3 μm, 4 mm x 150 mm column, mobile phase consisting of acetonitrile and water (65:35 V/V) and UV detection at 277 nm using a photodiode array detector in the stressed sample chromatograms. Crushed sirolimus tablets were exposed to thermal, photolytic, aqueous and oxidation stress conditions and stressed samples were analysed by the proposed method. Peak homogeneity data of the drug peaks were obtained using photodiode array detector. The stressed sample chromatograms demonstrated the specificity of the method for their estimation in presence of degradants. 99.66% degradation was observed in acid degradation study. on the other hand, no degradation was observed in aqueous condition. The given method was linear over a range of 0.1566 mg/mL to 0.4699 mg/mL. The mean recovery was found to be 99.23%. Acid degradant was separated by HPTLC and spectroscopic analysis was performed for the same.

scholarly journals HPLC Analysis of Kaempherol and Quercetin Derivatives Isolated by Different Extraction Techniques from Plant Matrix

2011 ◽  
Vol 94 (1) ◽  
pp. 17-21 ◽  
Author(s):  
Krystyna Skalicka-Woźniak ◽  
Janusz Szypowski ◽  
Kazimierz Głowniak
Keyword(s):  
Hplc Analysis ◽  
Soxhlet Extraction ◽  
Array Detector ◽  
Extraction Techniques ◽  
Ultrasound Extraction ◽  
Quercetin Derivatives ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Photodiode Array

Abstract Soxhlet extraction, ultrasound extraction, and accelerated solvent extraction (ASE), followed by RP-HPLC with a photodiode array detector was used for the determination of flavonoids in fruits of Peucedanum alsaticum. Three compounds were identified: a kaempherol derivative (astragalin), and two quercetin derivatives (quercitrin and hiperoside). The highest extraction yields of the selected compounds were obtained by use of exhaustive ASE.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR RILPIVIRINE HYDROCHLORIDE IN BULK AND USE IN ANALYSIS OF PREPARED NANOSUSPENSION

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (04) ◽  
pp. 42-46
Author(s):  
Madhuri Manchala ◽  
◽  
Vijaya Sri Kanagala ◽  
Ganapath Vinay Jain
Keyword(s):  
Homogenization Method ◽  
Hplc Method ◽  
Array Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation ◽  
Tablet Dosage

A simple, precise, accurate and robust RP-HPLC-PDA method was developed and validated for the determination of rilpivirine hydrochloride in tablet dosage forms. Reverse-phase chromatography was performed on a BDS hypersil (250 mm × 4.6 mm, 6 μm) column of Waters HPLC with Empower software and with a photodiode array detector. Methanol: acetonitrile: water 80:13.5:6.5 (v/v) was used as the mobile phase at a flow rate of 1 mL min-1 with PDA detection at 306 nm. Rilpivirine hydrochloride nanosuspension was prepared by using an ultrasonic homogenization method. Linearity was observed in the concentration range of 0.1–10 μg mL-1 with regression equation y = 508856X+46908 (R2 = 0.9998). The method was validated as per ICH guidelines. The RSD for intra-day (1.31- 0.67) and inter-day (1.69-1.59) precision was found to be less than 2%. The developed method is simple, precise and robust for the determination of rilpivirine hydrochloride and is successfully applied for the nanosuspension.

Method Development and Validation for the Determination of Linezolid Drug in Human Plasma by Reversed-Phase High-Performance Liquid Chromatography

2021 ◽  
Vol 17 ◽  
Author(s):  
Missoum Amina ◽  
Kahina Hamza ◽  
Fatiha Malki ◽  
Abderrezak Hamdi ◽  
Hassan Y. Aboul-Enein
Keyword(s):  
Particle Size ◽  
Flow Rate ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Pharmacokinetic Studies ◽  
Photodiode Array Detector ◽  
Photodiode Array

Objective: Linezolid is a significant antibiotic used against severe infections initiated by multi-resistant bacterial pathogens. Method: Linezolid extraction from plasma is obtained using methanol. Chromatographic separation is achieved isocratically on a C18 column [Zorbax C18, 5 µm particle size, 150 mm ˟ 4.6 mm] making use of a mobile phase of acetonitrile / 0.05 M phosphate buffer, pH = 4.5 (30 : 70 v/v) at a flow rate of 1.2 mL/min with photodiode array detector DAD, at a wavelength of 256 nm. Method: Linezolid extraction from plasma is obtained using methanol. Chromatographic separation is achieved isocratically on a C18 column [Zorbax C18, 5 µm particle size, 150 mm ˟ 4.6 mm] making use of a mobile phase of acetonitrile / 0.05 M phosphate buffer, pH = 4.5 (30 : 70 v/v) at a flow rate of 1.2 mL/min with photodiode array detector DAD, at a wavelength of 256 nm. Results : The retention time of linezolid was 2.5 min. The analytical method was linear (r2 > 0.998) over the calibration range of 0.30 to 50.0 µg/mL. The extraction recoveries of linezolid range from 71.03 to 91.93 %. The limit of quantification and the limit of detection were 0.112 µg and 0.037 µg, respectively. The RSDs for intraday and interday assays were < 7.77 and 4.32 %, respectively. The intraday and interday accuracies were in the range 80.6-112 % and 77.44-104.85 %, respectively. Conclusion: The applied method is precise, accurate and appropriate for pharmacokinetic studies and therapeutic drug monitoring of linezolid in routine clinical practice.

scholarly journals A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Ali S. Abdelhameed ◽  
Samar A. Afifi
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Rat Plasma ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Interday Precision

A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear withr2=0.9999for PTZ andr2=0.9995for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH) guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD) <7.76% for PTZ and <7.58 % for ETD.

scholarly journals A 100% Water Mobile Phase HPLC-PDA Analysis of Selected Neonicotinoid Insecticides

2014 ◽  
Vol 10 (9) ◽  
pp. 3127-3132
Author(s):  
Naoto Furusawa
Keyword(s):  
Mobile Phase ◽  
Detection Limits ◽  
Hplc Method ◽  
Array Detector ◽  
Acceptance Criteria ◽  
Chromatographic Separations ◽  
Neonicotinoid Insecticides ◽  
Photodiode Array Detector ◽  
System Suitability ◽  
Photodiode Array

This paper describes a reserved-phase HPLC method for detecting frequently-used neonicotinoid insecticides, acetamiprid (ATP) and imidacloprid (ICP), using an isocratic 100 % water mobile phase.  Chromatographic separations were performed an Inertsil® WP300 C4 with water mobile phase and a photodiode-array detector.  The total run time was < 7 min.  The system suitability was well within the international acceptance criteria.  The detection limits were 0.013 μg ml-1 for ATP and 0.015 μg ml-1 for ICP, respectively.  A harmless HPLC method for simultaneous detecting ATP and ICP was developed and may be further applied to the quantification in foods.  

scholarly journals DETERMINATION OF LUTEOLIN FROM EXTRACTIONS OF Helicteres hirsuta BY HPLC

2019 ◽  
Vol 128 (1B) ◽  
pp. 43
Author(s):  
Lê Trung Hiếu ◽  
Lê Lâm Sơn ◽  
Nguyễn Minh Nhung ◽  
Hồ Xuân Anh Vũ ◽  
Trần Thị Văn Thi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Array Detector ◽  
Plant Parts ◽  
Aerial Parts ◽  
Photodiode Array Detector ◽  
Photodiode Array

<p>High performance liquid chromatography coupled with photodiode array detector (HPLC- DAD) has been reported to quantify isolated compounds. This work was designed, therefore, to develop an HPLC-DAD system to determine luteolin in extractive solutions from <em>Helicteres hirsuta</em>. Luteolin was analyzed on a RP- C18 column, using a mobile phase including: acetonitrile - 0.1% acid phosphoric (v/v), under the following conditions detecting wavelength: 347 nm; flow rate: 0.5 mL/min, and the volume of injecting sample: 10 μL. The HPLC system was carried out at ambient temperature. The method showed linearity for luteolin in the range to 0.02 from 1 mg/mL, and the recovery of luteolin was 94.07 ± 0.64. Contents of  luteolin in methanol extracts from the plant parts of <em>H. hirsuta</em> (including: branch, leaf, fruit and aerial parts) were determined with value of 49.06 ±0.46, 142.89 ±0.53, 56.61±0.62 and 91.15±0.42 µg/g, respectively.</p>

scholarly journals Novel RP-HPLC-PDA Approach for Efficient Simultaneous Quantification of Imipenem, Cilastatin and Relebactum in Bulk Drug and Injection Dose Forms

2021 ◽  
Vol 33 (4) ◽  
pp. 897-902
Author(s):  
Krishnaphanisri Ponnekanti ◽  
K. Sunitha
Keyword(s):  
Target Range ◽  
Array Detector ◽  
Photodiode Array Detection ◽  
Rp Hplc ◽  
Dipotassium Hydrogen Phosphate ◽  
Photodiode Array Detector ◽  
Injection Dose ◽  
Photodiode Array ◽  
Bulk Drug ◽  
Inactive Ingredients

In this investigation, a highly reliable, precise, stability indicating, specific and selective RP-HPLC approach with photodiode array detection (RP-HPLC-PDA) was established to determine simultaneously imipenem, cilastatin and relebactum in bulk drug and injection dose forms. Chromatographic separation of imipenem, cilastatin and relebactum was achieved via using C18 XTerra column and a mobile phase poised of acetonitrile and 0.1 M dipotassium hydrogen phosphate buffer (4.5 pH, set with 0.1% orthophosphoric acid) at 45:55 (v/v) ratio with a flow stream of 1 mL/min. The photodiode array detector was fixed at wavelength 245 nm and quantifications of imipenem, cilastatin and relebactum were based on assessing their peak response areas. Good linearity was detected in target range concentrations of 250-750 μg/mL (imipenem and cilastatin) and 125-375 μg/mL (relebactum). The precision (standard variation percentage) was between 0.141% and 0.257%. Accuracy (%assay nominal) determined was between 99.144% and 99.638%. The validated RP-HPLC approach was applied to Recarbio injection dose evaluating imipenem, cilastatin and relebactum content with no interference encountered from the injection dose inactive ingredients. Imipenem, cilastatin and relebactum were subjected to forced conditions like 30% peroxide, 0.1 N NaOH, sunlight, 0.1 N HCl and 60 ºC. Imipenem, cilastatin and relebactum were effectively separated, quantified and resolved from the degradants generated in forced conditions.

scholarly journals Determination of xanthophylls compounds in dietary supplements by HPLC-PDA

2019 ◽  
Vol 2 (2) ◽  
pp. 51-56
Author(s):  
Thanh Hoa Mac Thi ◽  
Hong Ngoc Nguyen Thi ◽  
Mai Hoa Duong Thi ◽  
Khanh Cao Cong ◽  
◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Dietary Supplements ◽  
Mobile Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Linear Calibration ◽  
Chromatography Column ◽  
Photodiode Array Detector ◽  
Photodiode Array

An HPLC method using photodiode array detector (PDA) detector has been developed for the&nbsp;determination of astaxanthin, lutein, and zeaxanthin in dietary supplements. These compounds&nbsp;were separated on a C30 chromatography column with ethyl acetate: acetonitrile (12:88, v/v)&nbsp;containing 0.1% n-decanol as the mobile phase. Xanthophyll compounds, usually existing in the&nbsp;form of esters, were saponified in 45% KOH solution (with lutein and zeaxanthin) and 1% (with&nbsp;astaxanthin) at 60&deg;C within 15 minutes, then re-extracted with n-hexane before analyzing on HPLC&nbsp;system. The method was validated and had good specificity and selectivity. The linear calibration&nbsp;curve in the range of 0.5 - 10 &micro;g/ml, the repeatability and the recovery of the method meet the analytical&nbsp;requirements according to AOAC; the method was applied to analyze several dietary supplements&nbsp;collected from market.

Simultaneous Determination of Co-administrated Deflazacort, Aprepitant and Granisetron in Dosage Forms and Spiked Human Plasma by RP-HPLC/PAD

2019 ◽  
Vol 57 (9) ◽  
pp. 790-798 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Soheir Alweshahy ◽  
Dalia A Elshabasy ◽  
Nadia F Youssef
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Array Detector ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array

Abstract A selective reversed phase high performance liquid chromatography/photodiode array detector (RP-HPLC/PAD) method has been developed for simultaneous determination of the three co-administrated deflazacort, aprepitant and granisetron drugs used with chemotherapy. The three cited drugs have been chromatographed on C18 column using a mobile phase consisting of acetonitrile–0.2% v/v triethylamine (80:20 v/v, pH of 6.6 ± 0.05) with isocratic elution and monitored by photodiode array at 220 nm. International conference on harmonization (ICH) guidelines were followed to validate the developed method. Successful application of the developed method was assessed by the simultaneous determination of the studied drugs in pure forms, dosage forms and plasma samples in the ranges of 0.2–20, 0.4–40 and 0.2–20 μg/mL for deflazacort, aprepitant and granisetron, respectively.

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