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 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.

scholarly journals Development of a Validated Stability Indicating Method for Quantification of Amoxicillin, Clarithromycin and Lansoprazole in Bulk and Pharmaceutical Dosage form by RP-HPLC

2021 ◽  
pp. 207-220
Author(s):  
P. Sushma ◽  
A. K. M. Pawar ◽  
M. Divya
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
System Suitability ◽  
Photodiode Array

Objective: The main objective of the present work is to develop an efficient, unique, reliable Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method for the simultaneous quantification of Amoxicillin (AMX), Clarithromycin (CTM) and Lansoprazole (LPZ) in bulk and pharmaceutical formulations.  Methods: The chromatographic separation was achieved by using Kinetex column C18 (100 x 4.6 mm, 2.6 µm) with Buffer (2.5 g of hexane sulphonic acid and 1ml of Triethylamine which are added to 1000 ml of HPLC water and adjusted its pH at 5.0 with Ortho phosphoric acid) and acetonitrile in the ratio of 70: 30 (%v/v) as a mobile phase at flow rate of 1.0 ml/min. The column effluents were monitored by a photodiode array detector at wavelength predetermined at 240 nm. Results: The method produced reliable results at optimized chromatographic conditions. The method was linear at concentration range of 15-225 µg/ml of AMX, 15-225 µg/ml of CTM and 0.9-13.5 µg/ml of LPZ with regression coefficients of 0.9999, 0.9999, and 0.9999 respectively. The retention times of AMX, CTM, LPZ were obtained as 1.513, 3.124, 3.770 min respectively. Results obtained for system suitability, precision, LOD and LOQ were in acceptable range and were validated according to the guidelines of the International Council for Harmonization (ICH). Conclusion: The proposed method was validated in accordance with ICH and all the obtained results were found satisfactory and were successfully applicable to the analysis of the bulk and the pharmaceutical formulations.

Development and Validation of an HPLC Method for Determination of Spirotetramat and Spirotetramat cis enol in Various Vegetables and Soil

2013 ◽  
Vol 96 (3) ◽  
pp. 670-675 ◽  
Author(s):  
Balwinder Singh ◽  
Kousik Mandal ◽  
Sanjay K Sahoo ◽  
Urvashi Bhardwaj ◽  
Raminderjit Singh Battu
Keyword(s):  
Analytical Method ◽  
Anhydrous Sodium Sulfate ◽  
Hplc Method ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Precision And Accuracy ◽  
Hplc Grade Acetonitrile ◽  
Development And Validation

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

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 SIMULTANEOUS QUANTIFICATION OF PENTAZOCINE AND NALOXONE BY STABILITY INDICATING REVERSE-PHASE-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD

2019 ◽  
pp. 257-262
Author(s):  
RAMA KUMAR KANDULA ◽  
RAJA SUNDARARAJAN
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Alkali Hydrolysis ◽  
Liquid Chromatographic

Objective: The objective of the study was to develope a stability indicating high-performance liquid chromatographic (HPLC) method for simultaneous assay of pentazocine and naloxone in bulk and tablets. Methods: Pentazocine and naloxone were analyzed on Dionex C18 column using 0.1M K2HPO4 buffer (pH 4.0) and methanol (60:40, v/v) as the mobile phase. The concentration of pentazocine and naloxone was quantified by photodiode array detector set at 248 nm. The method was validated in compliance with ICH rules. Pentazocine and naloxone tablet formulation was subjected to forced degradation such as acid, neutral and alkali hydrolysis, oxidation, photo, and thermal degradation. Results: The method was linear, with R2=0.9999 in the concentration range 100–300 μg/ml for pentazocine and R2=0.9995 in the concentration range 1–3 μg/ml for naloxone. The level of detection and quantification was 0.097 μg/ml and 0.322 μg/ml for pentazocine and 0.0073 μg/ml and 0.0243 μg/ml for naloxone, respectively. The degraded products are resolved well from pentazocine and naloxone with significantly different retention time values. From validation results, it was proved that the method is selective, precise, robust, and accurate for the estimation of pentazocine and naloxone simultaneously. Conclusion: The developed stability-indicating HPLC method can be applied for quantitative determination of pentazocine and naloxone in tablets.

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.

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