scholarly journals Development and Validation of a Method for Ionic Dyes Determination in Guava Fibrous Matrix Using Reverse Phase Chromatography

2021 ◽  
Author(s):  
Marina dos Reis ◽  
Fabiano Silva ◽  
Fernando Madureira ◽  
Eugênia Vargas ◽  
Lucas Oliveira ◽  
...  
Keyword(s):  
Simple Procedure ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Simple Method ◽  
Reverse Phase Chromatography ◽  
Fibrous Matrix ◽  
Food Dyes ◽  
Initial Ph ◽  
Orange G ◽  
Development And Validation

In this work, a method for food dyes determination in fibrous fruit pulps was developed. The analytes Tartrazine, Twilight Yellow FCF, Erythrosine, Orange G and Allura Red were analyzed by reverse phase chromatography with diode array (DAD) detection. The sample preparation consisted of a simple procedure, based on initial pH adjustment of the sample (pH = 10.0), followed by an extraction with acetonitrile (5.0 mL and agitation for 30 s), ultrasonic (5 min) and centrifugation (4000 rpm, 20 ºC, for 20 min). The supernatant had its pH adjusted to 3.0, followed by filtration. The method was validated, with the analytical curves prepared in a matrix, in the range of 50 to 150 mg kg-1 for all the analytes studied (determination coefficients (R2) > 0.99). The method veracity was evaluated in terms of recovery, obtaining recoveries of 93-110%. The repeatability was less than 13.7%, while the intermediate precision was less than 19.0%. The limits of detection and quantification were determined, being 15 and 30 mg kg-1, respectively. The combined relative uncertainties were less than 13.8%. Therefore, it can be concluded that a simple method was developed, suitable for monitoring the presence of dyes in fruit pulps in routine analyzes.

scholarly journals Development and Validation of RP-LC Method for the Determination of Cinnarizine/Piracetam and Cinnarizine/Heptaminol Acefyllinate in Presence of Cinnarizine Reported Degradation Products

2013 ◽  
Vol 8 ◽  
pp. ACI.S12478 ◽  
Author(s):  
Ola M. EL-Houssini ◽  
Nagwan H. Zawilla ◽  
Mohammad A. Mohammad
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Reverse Phase Liquid Chromatography ◽  
Phase Liquid ◽  
Development And Validation

Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20-200, 20-1000 and 25-1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations.

scholarly journals A simple method for the quantification of diclofenac potassium in oral suspension by high-performance liquid chromatography with UV-detection

2013 ◽  
Vol 49 (3) ◽  
pp. 589-597 ◽  
Author(s):  
Alexandre Machado Rubim ◽  
Jaqueline Bandeira Rubenick ◽  
Luciane Varine Laporta ◽  
Clarice Madalena Bueno Rolim
Keyword(s):  
High Performance ◽  
Low Cost ◽  
Oral Suspension ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Simple Method ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Validation Parameters

A rapid, simple and low cost method was developed to determine diclofenac potassium (DP) in oral suspension, using a reverse-phase column (C8, 150 mm x 4.6 mm, 5 µm), mobile phase containing methanol/buffer phosphate (70:30 v/v, pH 2.5), at a flow rate of 1.0 mL/min, isocratic method, and ultraviolet detection at 275 nm. A linear response (r = 1.0000) was observed in the range of 10.0-50.0 µg/mL. Validation parameters such as linearity, specificity, precision, accuracy and robustness were evaluated. The method presented precision (repeatability: relative standard deviation = 1.21% and intermediate precision: between-analyst = 0.85%). The specificity of the assay was evaluated by exposure of diclofenac potassium under conditions of stress such as hydrolysis, photolysis, oxidation and high temperature. The method presented accuracy values between 98.28% and 101.95%. The results demonstrate the validity of the proposed method that allows determination of diclofenac potassium in oral suspension and may be used as an alternative method for routine analysis of this product in quality control.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Benzimidamidecontent) in Leflunomide by Using RP-HPLC Technique

2021 ◽  
pp. 78-85
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Program Mode

The measurement of Genotoxic contaminant, a simple, selective, linear, accurate, and specific reverse phase high-performance liquid chromatographic (RP-HPLC) process was proposed. A Benzimidamide impurity in the medication Leflunomide has been discovered. Separation and analysis were carried out on Zorbax SB phenyl (4.6 mm x 250 mm) with a particle size of 5.0 μm. with 0.1 % Triethylamine in purified water with a pH of 7.0 and a buffer of phosphoric acid (20% in water). The mobile phase is a 40:60 mixture of buffer and Acetonitrile with degassing. Isocratic program mode was used. The elution was carried out at a rate of 1.0 mL/min with UV detection at a wavelength of 289 nm. The temperature of the selected column oven is 25°C. The linearity and accuracy of Benzimidamide are covered in this approach, with a LOQ limit of 150 percent (i.e.0.03 to 0.45 ppm). The observed correlation coefficient is 0.99994, with a range of 100.01 to 104.8 for recovery. The measured percent RSD of six spiked test preparation is below 5.0 percent in procedure precision (i.e. repeatability) and intermediate precision (IP). When maintained at room temperature, the standard and sample remained stable for three days. System appropriateness characteristics such as tailing factor and percent RSD do not exhibit significant changes in robustness experiments. For the detection of Benzimidamide the present RP-HPLC method is act as selective, robust, linear and precise.

scholarly journals Development and Validation of 2-Azaspiro [4,5] Decan-3-One (Impurity A) in Gabapentin Determination Method Using qNMR Spectroscopy

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1656
Author(s):  
Nataliya E. Kuz’mina ◽  
Sergey V. Moiseev ◽  
Mikhail D. Khorolskiy ◽  
Anna I. Lutceva
Keyword(s):  
Test Procedure ◽  
Active Pharmaceutical Ingredient ◽  
Test Methods ◽  
Intermediate Precision ◽  
Coefficients Of Variation ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Student’S T ◽  
Development And Validation ◽  
Student’S T Test

The authors developed a 1H qNMR test procedure for identification and quantification of impurity A present in gabapentin active pharmaceutical ingredient (API) and gabapentin products. The validation studies helped to determine the limit of quantitation and assess linearity, accuracy, repeatability, intermediate precision, specificity, and robustness of the procedure. Spike-and-recovery assays were used to calculate standard deviations, coefficients of variation, confidence intervals, bias, Fisher’s F test, and Student’s t-test for assay results. The obtained statistical values satisfy the acceptance criteria for the validation parameters. The authors compared the results of impurity A quantification in gabapentin APIs and capsules by using the 1H qNMR and HPLC test methods.

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 Optical Methods for Zeta Potential Determination of Silica and Polystyrene Particles in Aqueous Suspensions

Materials ◽  
2021 ◽  
Vol 14 (2) ◽  
pp. 290
Author(s):  
Yannic Ramaye ◽  
Marta Dabrio ◽  
Gert Roebben ◽  
Vikram Kestens
Keyword(s):  
Zeta Potential ◽  
Particle Tracking ◽  
Colloidal Stability ◽  
Optical Methods ◽  
Intermediate Precision ◽  
Electrophoretic Light Scattering ◽  
Measurement Uncertainties ◽  
Development And Validation ◽  
Direct Implementation

Zeta potential is frequently used to examine the colloidal stability of particles and macromolecules in liquids. Recently, it has been suggested that zeta potential can also play an important role for grouping and read-across of nanoforms in a regulatory context. Although the measurement of zeta potential is well established, only little information is reported on key metrological principles such as validation and measurement uncertainties. This contribution presents the results of an in-house validation of the commonly used electrophoretic light scattering (ELS) and the relatively new particle tracking analysis (PTA) methods. The performance characteristics were assessed by analyzing silica and polystyrene reference materials. The ELS and PTA methods are robust and have particle mass working ranges of 0.003 mg/kg to 30 g/kg and 0.03 mg/kg to 1.5 mg/kg, respectively. Despite different measurement principles, both methods exhibit similar uncertainties for repeatability (2%), intermediate precision (3%) and trueness (4%). These results confirm that the developed methods can accurately measure the zeta potential of silica and polystyrene particles and can be transferred to other laboratories that analyze similar types of samples. If direct implementation is impossible, the elaborated methodologies may serve as a guide to help laboratories validating their own methods.

Sign in / Sign up

Export Citation Format

Share Document