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.

scholarly journals Development and Validation of a Column High-Performance Liquid Chromatography Method for Quantification of Ganaphaliin A and B in Inflorescences of Gnaphalium liebmannii Sch. Bp ex Klatt

2011 ◽  
Vol 94 (4) ◽  
pp. 1076-1081 ◽  
Author(s):  
Fernando Rodríguez-Ramos ◽  
Víctor H Sánchez-Estrada ◽  
Alejandro Alfaro-Romero ◽  
Gabriela Rubí Tapia-Álvarez ◽  
Andrés Navarrete
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Raw Material ◽  
Array Detector ◽  
Chromatography Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatography Method ◽  
Development And Validation

Abstract An HPLC method was developed for the simultaneous determination of gnaphaliin A and B, active compounds of Gnaphalium liebmannii Sch. Bp ex Klatt. The HPLC separation was performed on an Inertsil ODS-3 (150 × 4.6 mm id, 5 μm) RP C18 column operated at 40°C; the isocratic mobile phase was 0.02% aqueous orthophosphoric acid– methanol–acetonitrile (50 + 30 + 20, v/v/v), with a run time of 20 min and flow rate of 1.5 mL/min. Detection with a photodiode array detector (PDAD) was at 270 nm. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ for gnaphaliin A and B were found to be in the range of 0.4–0.5 and 1.0–1.4 μg/mL, respectively. This is the frst report of an analytical method developed for the quantitative analysis of flavones from Gnaphalium species by HPLC-PDAD with applications for raw material and commercial products.

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.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

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.

scholarly journals Development and validation of indocyanine green assay in human plasma using High-Performance Liquid Chromatography with PDA detector

2019 ◽  
Vol 10 (2) ◽  
pp. 1007-1012
Author(s):  
Sumith K Mathew ◽  
Blessed Winston A ◽  
Aswathy Mathew ◽  
Jeana Jacob ◽  
Ratna Prabha ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Indocyanine Green ◽  
High Performance ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Blood Specimens ◽  
Development And Validation

A robust and economical assay for routine determination of indocyanine green pharmacokinetics was developed and validated using high-performance liquid chromatography with a photodiode array detector. Plasma specimens from critically ill patients and those with hepatitis on various co-medications were used as blanks for validation of this assay. Extraction of indocyanine green was performed by simple protein precipitation with acetonitrile, and the supernatant was separated using an octadecyl column with detection at 784 nm. Blanks were found to have no interference for 40 blanks of patients who were on 56 different medications. The precision for LLOQ (0.5 µg/ml) as determined by the percentage coefficient of variation was 1.19. Stability of plasma calibration standards and stock were determined over a period of 61 days, and ICG was found to be stable for 20 days. Stability of whole blood specimens containing ICG was determined at 4°C for a period of 4 hours.

A Novel HPLC Method for Simultaneous Determination of Methyl, Ethyl, n-propyl, Isopropyl, n-butyl, Isobutyl and Benzyl Paraben in Pharmaceuticals and Cosmetics

2020 ◽  
Vol 23 ◽  
Author(s):  
Saniye Özcan ◽  
Serkan Levent ◽  
Nafiz Öncü Can
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Methyl Ethyl ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatographic

: The alkyl esters of p-hydroxybenzoic acid at the C-4 position, “the parabens,” including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure. On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methyl paraben (MP), ethyl paraben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products. The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%. The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six of the samples, and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples is 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.

scholarly journals Determination of Tadalafil in Pure Powder and Tablet Dosage Form by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (2) ◽  
pp. 516-522 ◽  
Author(s):  
Tushar G Barot ◽  
Popatbhai K Patel
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Degradation Products ◽  
Accurate Method ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Tablet Dosage ◽  
Isocratic Mode

Abstract A simple and accurate method to determine tadalafil (TAD) in pure powder and tablet dosage form was developed and validated using HPLC. The separation was achieved on an Xterra RP18 column (150 4.6 mm id, 3.5 m) in the isocratic mode using bufferacetonitrile (70 + 30, v/v), adjusted to pH 7.00 0.05 with triethylamine as the mobile phase at a flow rate of 1.0 mL/min. The photodiode array detector was set at 225 nm. Quantification was achieved over the concentration range of 50.7152.10 g/mL with mean recovery of 100.26 0.75. The method was validated and found to be simple, accurate, precise, and specific. The method was successfully applied for the determination of TAD in pure powder and tablet dosage form without interference from common excipients or degradation products.

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.

scholarly journals Development and validation of an HPLC method for the determination of fluorouracil in polymeric nanoparticles

2013 ◽  
Vol 49 (1) ◽  
pp. 117-126 ◽  
Author(s):  
Ana Cristina de Mattos ◽  
Najeh Maissar Khalil ◽  
Rubiana Mara Mainardes
Keyword(s):  
Quantitative Analysis ◽  
Flow Rate ◽  
High Performance ◽  
Polymeric Nanoparticles ◽  
Hplc Method ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Relative Standard ◽  
Photodiode Array ◽  
Development And Validation

The objective of this work was to develop and validate a rapid high performance liquid chromatography (HPLC) method for the quantitative analysis of fluorouracil (5-FU) in polymeric nanoparticles. Chromatographic analyses were performed on an RP C18 column with a mobile phase consisting of acetonitrile and water (10:90, v/v) at a flow rate of 1 mL/min. The 5-FU was detected and quantitated using a photodiode array detector at a wavelength of 265 nm. The method was shown to be specific and linear in the range of 0.1-10 µg/mL (r = 0.9997). The precision (intra- and inter-day) was demonstrated because the maximum relative standard deviation was 3.51%. The method is robust relative to changes in flow rate, column and temperature. The limits of detection and quantitation were 10.86 and 32.78 ng/mL, respectively. The method fulfilled the requirements for reliability and feasibility for application to the quantitative analysis of 5-FU in polymeric nanoparticles.

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