Development and validation of a short runtime method for separation of trace amounts of 4-aminophenol, phenol, 3-nitrosalicylic acid and mesalamine by using HPLC system

In a short runtime process (about 6 minutes), with isocratic method without need of reconditioning before the next run, a mixture of some molecules containing 4-aminophenol (4APh), phenol, 3-nitrosalicylic acid (3NSA), and mesalamine (5-aminosalicylic acid) (MLZ), were separated and detected by means of HPLC/UV-Vis system. The resolutions of the separated and sharp peaks referring to the mentioned compounds were at least more than 2, and the tailing factor (TF) was about 1, even in 1 µg/l (ppm) concentration. In order to optimize the method, the effects of the pH, eluent percentage, flow rate, and buffer concentration, and wavelength on the chromatogram were investigated. Also, the results of the validation processes showed that the method trustable to be used in laboratories.

Development and Validation of RP-HPLC Method for Analysis of Aclidinium Bromide and Formoterol Fumarate in Pharmaceuticals

Asian Journal of Pharmaceutical Analysis ◽

10.52711/2231-5675.2021.00012 ◽

2021 ◽

pp. 63-69

Author(s):

Devadasu Ch ◽

Bharani V

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Hplc Method ◽

Rp Hplc ◽

Hplc System ◽

Standard Procedures ◽

Aclidinium Bromide ◽

Formoterol Fumarate

A fast, sensitive, and reliable RP-HPLC method involving cyberlab HPLC System with PDA detection was developed and validated for the quantification of Aclidinium bromide and Formoterol fumarate in inhalation preparations. Chromatography was performed on the Inertsil -ODS C18 (250 x 4.6mm, 5μ) column using filtered and mixed degassed methanol: buffer (75:25 v/v) as a mobile phase with a flow rate of 1.0mL/min and the column effluent was monitored at 240nm. Retention times for Aclidinium bromide 4.713min and Formoterol fumarate 6.691min. The method obeyed linearity in the concentration range of 20-80µg/mL for the two drugs when validated according to standard procedures.

Development and validation of a rapid selective high-throughput LC-MS/MS method for the determination of triclabendazole sulfoxide concentrations in sheep plasma and its use in bioequivalence studies

Acta Chromatographica ◽

10.1556/1326.2021.00891 ◽

2021 ◽

Author(s):

Lénárd Farczádi ◽

Álmos Dósa ◽

Orsolya Melles ◽

Laurian Vlase

Keyword(s):

Formic Acid ◽

Flow Rate ◽

Mobile Phase ◽

Liver Fluke ◽

Internal Standard ◽

Gradient Elution ◽

Sample Processing ◽

Analytical Separation

AbstractTriclabendazole is one of the main drugs used to treat liver fluke in livestock. A rapid LC-MS/MS method was developed and validated to determine ovine plasma levels of triclabendazole sulfoxide.A Gemini NX-C18 column was used to achieve analytical separation, with gradient elution of a mobile phase composed of 0.1% formic acid in acetonitril and 0.1% formic acid in water at flow rate of 0.6 mL/min. MRM with positive ESI ionization was used for the detection of triclabendazole sulfoxide (m/z 360.10 from m/z 376.97). Fenbendazole was used as internal standard. Plasma protein precipitation with acetonitrile was used for sample processing.The method was validated with regards to selectivity, linearity (r > 0.9939), within run and between run precision (CV < 8.9%) and accuracy (bias < 8.9%) over the concentration range 1–100 µg/mL plasma.The method developed is simple, selective and can be applied in bioequivalence and bioavailability studies.

Development and Validation of RP-HPLC for Estimation of Neratinib in Bulk and Tablet Dosage Form

International Journal of Pharmaceutical Sciences and Drug Research ◽

10.25004/ijpsdr.2019.110202 ◽

2019 ◽

Vol 11 (02) ◽

Author(s):

M Lakshmi Kanth ◽

B Raj Kama

Keyword(s):

Flow Rate ◽

Retention Time ◽

Chromatographic Separation ◽

Mobile Phase ◽

Dosage Form ◽

Hplc Method ◽

Rp Hplc ◽

Monopotassium Phosphate ◽

Tablet Dosage

An accurate RP-HPLC method developed for the estimation of Neratinib in bulk and tablet dosage form. The method is and validated for parameters linearity, accuracy, suitability, specificity, precession, LOD, LOQ and robustness. An Altima column (150 mm × 4.6 mm × 5μ) used for chromatographic separation within a runtime of 6 min. The mobile phase buffer (monopotassium phosphate) and acetonitrile (60:40 v/v) with 0.1% formic acid is used. The flow rate maintained at 1.0 ml/min with the effluents monitored at 215 nm. The Neratinib analyzed at retention time of 4.001. The concentration linear over 30-180μg/ml with regression equation y = 6065.6x + 795.43 and regression co-efficient 0.999.

QbD Approach for the Development and Validation of RP-UHPLC Method for Quantitation of Vildagliptin

Dhaka University Journal of Pharmaceutical Sciences ◽

10.3329/dujps.v16i1.33388 ◽

2017 ◽

Vol 16 (1) ◽

pp. 107-117

Author(s):

Sharifa Sultana ◽

Uttom Kumar ◽

Md Shahadat Hossain ◽

Dilshad Noor Lira ◽

Abu Shara Shamsur Rouf

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Quality By Design ◽

Response Surfaces ◽

Routine Analysis ◽

Pharmaceutical Dosage Forms ◽

Independent Variables ◽

Two Factors ◽

Bulk Drug ◽

The present work describes a quality by design (QbD)-based rapid, simple, precise and robust RPUHPLC method for the routine analysis of vildagliptin in bulk drug and in pharmaceutical dosage forms. Chromatographic separation was achieved by a X-bridge C18 column with isocratic elution of mobile phase containing mixture of phosphate buffer (pH 6.8) and acetonitrile in the ratio of 67:33(v/v). The flow rate was 1.0 ml/min and the detection was done at 239 nm with photo-diode array plus (PDA+) detector. The optimization of chromatographic method was carried out by QbD approach using design of experiments (DoE). Two factors utilized for the experimental design of the method were (i) independent variables which comprise percentages of acetonitrile in mobile phase and flow rate and (ii) co-variates which include the retention time, tailing factor and theoretical plates. This design was statistically analyzed by ANOVA, normal plot of residual, box-cox plot for power transform, perturbation, counter plot and 3D response surfaces plots. This was further validated as per the requirements of ICHQ2B guidelines for linearity, LOD, LOQ, accuracy, precision, specificity and robustness. The results showed that proposed method is simple, sensitive and highly robust for routine analysis of vildagliptin.Dhaka Univ. J. Pharm. Sci. 16(1): 107-117, 2017 (June)

Development and validation of a patient face-mounted, negative-pressure antechamber for reducing exposure of healthcare workers to aerosolized particles during endonasal surgery

Journal of Neurosurgery ◽

10.3171/2020.10.jns202745 ◽

2021 ◽

pp. 1-8

Author(s):

Mark Lee ◽

Hazel T. Rivera-Rosario ◽

Matthew H. Kim ◽

Gregory P. Bewley ◽

Jane Wang ◽

...

Keyword(s):

Flow Rate ◽

Negative Pressure ◽

High Speed ◽

Surgical Simulation ◽

Class I ◽

Physical Parameters ◽

Particle Sizing ◽

Aerosol Generation ◽

Open Face ◽

OBJECTIVE The authors developed a negative-pressure, patient face-mounted antechamber and tested its efficacy as a tool for sequestering aerated particles and improving the safety of endonasal surgical procedures. METHODS Antechamber prototyping was performed with 3D printing and silicone-elastomer molding. The lowest vacuum settings needed to meet specifications for class I biosafety cabinets (flow rate ≥ 0.38 m/sec) were determined using an anemometer. A cross-validation approach with two different techniques, optical particle sizing and high-speed videography/shadowgraphy, was used to identify the minimum pressures required to sequester aerosolized materials. At the minimum vacuum settings identified, physical parameters were quantified, including flow rate, antechamber pressure, and time to clearance. RESULTS The minimum tube pressures needed to meet specifications for class I biosafety cabinets were −1.0 and −14.5 mm Hg for the surgical chambers with (“closed face”) and without (“open face”) the silicone diaphragm covering the operative port, respectively. Optical particle sizing did not detect aerosol generation from surgical drilling at these vacuum settings; however, videography estimated higher thresholds required to contain aerosols, at −6 and −35 mm Hg. Simulation of surgical movement disrupted aerosol containment visualized by shadowgraphy in the open-faced but not the closed-faced version of the mask; however, the closed-face version of the mask required increased negative pressure (−15 mm Hg) to contain aerosols during surgical simulation. CONCLUSIONS Portable, negative-pressure surgical compartments can contain aerosols from surgical drilling with pressures attainable by standard hospital and clinic vacuums. Future studies are needed to carefully consider the reliability of different techniques for detecting aerosols.

Development and Validation of LC Method for the Determination of Famciclovir in Pharmaceutical Formulation Using an Experimental Design

E-Journal of Chemistry ◽

10.1155/2008/858462 ◽

2008 ◽

Vol 5 (1) ◽

pp. 58-67 ◽

Cited By ~ 3

Author(s):

Srinivas Vishnumulaka ◽

Narasimha Rao Medicherla ◽

Allam Appa Rao ◽

G. Edela Srinubabu

Keyword(s):

Experimental Design ◽

Flow Rate ◽

Mobile Phase ◽

Internal Standard ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Internal Standard Method ◽

Intermediate Precision ◽

Mobile Phase Flow Rate ◽

A rapid and sensitive RP-HPLC method with UV detection (242 nm) for routine analysis of famciclovir in pharmaceutical formulations was developed. Chromatography was performed with mobile phase containing a mixture of methanol and phosphate buffer (50:50,v/v) with flow rate 1.0 mL min−1. Quantitation was accomplished with internal standard method. The procedure was validated for linearity (correlation coefficient =0.9999), accuracy, robustness and intermediate precision. Experimental design was used for validation of robustness and intermediate precision. To test robustness, three factors were considered; percentage v/v of methanol in mobile phase, flow rate and pH; flow rate, the percentage of organic modifier and pH have considerable important effect on the response. For intermediate precision measure the variables considered were: analyst, equipment and number of days. The RSD value (0.86%,n=24) indicated an acceptable precision of the analytical method. The proposed method was simple, sensitive, precise, accurate and quick and useful for routine quality control.

DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD OF 3, 4-METHYLENEDIOXY-N-ETHYLAMPHETAMINE IN DRIED BLOOD SPOT USING GAS CHROMATOGRAPHY-MASS SPEC-TROMETRY

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2020v12i4.32304 ◽

2020 ◽

pp. 94-99

Author(s):

YAHDIANA HARAHAP ◽

HANZEL IRAWAN ◽

KUSWARDANI

Keyword(s):

Flow Rate ◽

Analytical Method ◽

Method Development ◽

Internal Standard ◽

Mobile Phase Flow Rate ◽

Column Temperature ◽

Mass Spec ◽

Validation Criteria ◽

Blood Spot

Objective: This study aims to develop and validate the analytical method to determine 3,4-Methylenedioxy-N-ethylamphetamine (MDEA) in DBS using GC-MS. Methods: This research used liquid-liquid micro-extraction for sample preparation and analysis was performed by GC-MS. In the method development, the optimized parameters were flow rate, column temperature, the spot of blood volume, % haematocrit, extraction and reconstitution of solvent volume, and sonication duration. Validation of the chosen method was performed based on EMEA bioanalytical guideline in 2011. Results: The optimum chromatographic conditions were obtained using HP-5 MS capillary columns (30 m x 0.25 mm i.d; 0.25 μm ); helium with 99.9% purity as a mobile phase; flow rate of 1.0 ml/min; column temperature was 250 °C; MS detection using 4 fragments at m/z values of 72.00 and 44.00 for MDEA and 58.00 and 77.00 for ephedrine HCl as an internal standard. The DBS paper with the volume of blood spot 40 μl was then extracted using liquid-liquid micro-extraction with methanol 700 μl, sonication for 5 min, evaporated with nitrogen gas then reconstituted with 50 μl ethyl acetate. The validation results fulfilled the requirements based on the EMEA bioanalytical guideline in 2011. Conclusion: It can be concluded that the optimum condition of the analytical method by using GC-MS was obtained and fulfilled validation criteria with a range concentration of 15-250 ng/ml.

DEVELOPMENT AND VALIDATION OF A FAST AND SENSITIVE UHPLC-PDA METHOD FOR THE QUANTIFICATION OF URSOLIC ACID IN POLY(L-LACTIC ACID) NANOCAPSULES

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2020.v13i9.38993 ◽

2020 ◽

pp. 161-165

Author(s):

BRUNA CARLETTO ◽

AMANDA MARTINEZ LYRA ◽

ADRIANA YURIKO KOGA ◽

ANDRESSA NOVATSKI ◽

RUBIANA MARA MAINARDES ◽

...

Keyword(s):

Lactic Acid ◽

Ursolic Acid ◽

Flow Rate ◽

Mobile Phase ◽

High Performance ◽

Limits Of Detection ◽

Column Temperature ◽

Relative Standard ◽

Detection And Quantification

Objective: The aim of the present study is to develop and validation of a ultra-high performance liquid chromatography (UHPLC) method to determine the ursolic acid content and its encapsulation efficiency (EE) in lipid-core nanocapsules prepared from poly (L-lactic acid). Methods: A simple UHPLC-PDA method was developed and validated for the quantitative determination of ursolic acid in poly(L-lactic acid) nanocapsules. The chromatographic conditions used were: RP-C18 column, isocratic mobile phase containing acetonitrile:water (92:8, v/v), flow rate of 0.8 ml/min, column temperature of 50°C, and detection at 203 nm. The following parameters were evaluated: Specificity, linearity, limits of detection and quantification, precision, accuracy, and robustness. Results: The method was specific to the ursolic acid and linear (r=0.9998) in the range of 10–100 μg/ml. The limits of detection and quantification were 1.35 and 4.10 μg/ml, respectively. The precision was demonstrated by a relative standard deviation less than 2%. Adequate accuracy (98.35%±0.82) was obtained. Changes in flow rate, mobile phase, and column temperature did not significantly alter the peak area and the retention time of the ursolic acid. The mean EE was 99.89%. Conclusion: The method proved to be fast, sensitive, and simple for quantifying ursolic acid in nanocapsules and was successfully used for determining the EE.

Reverse-phase High-Performance Liquid Chromatography Method Development and Validation for Estimation of Glimepiride in Bulk and Tablet Dosage Form

International Journal of Pharmaceutical Quality Assurance ◽

10.25258/10.25258/ijpqa.11.2.18 ◽

2020 ◽

Vol 11 (02) ◽

pp. 296-302

Author(s):

Aseem Kumar ◽

Anil Kumar Sharma ◽

Rohit Dutt

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Flow Rate ◽

Retention Time ◽

Mobile Phase ◽

High Performance ◽

Hplc Method ◽

Reverse Phase ◽

Rp Hplc ◽

The present work demonstrates a simple, rapid, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method for analyzing glimepiride in pure and tablet forms. The present method was developed using a C18 column 150 × 4.6 mm, with 5 μm, and packing L1 maintained at a temperature of 30°C. The mobile phase was prepared by dissolving 0.5 gram of monobasic sodium phosphate in 500 mL of distilled water, pH of the solution adjusted to 2.1 to 2.7 with 10% phosphoric acid, and added 500 mL of acetonitrile. The mobile phase was pumped in the highperformance liquid chromatography (HPLC) system at a flow rate of 1 mL/min, and separation was carried out at 228 nm, using an ultraviolet (UV) detector. The chromatographic separation was achieved with peak retention time (RT) at about 9.30 minutes, and the method was found to be linear over a concentration range of 40 to 140 μg/mL. The specificity of the method represented no interference of the excipients during the analysis, and stability testing after 24 hours also showed that the method is suitable and specific. The accuracy was between 99.93 to 99.96%, with limit of detection (LOD) and limit of quantitation (LOQ) being 0.354 μg/mL, 1.18 μg/mL, respectively. Satisfactory results were found for precision and robustness parameters during the development and validation stage for the analytical method. The proposed method was also adopted for the analysis of glimepiride tablets to improve the overall quality control. Using this method, symmetric peak shape was obtained with reasonable retention time. The retention time of glimepiride for six repetitions is 9.3 ± 0.1 minutes; the run time is 21 minutes. The proposed RP-HPLC method is a modification of the United States Pharmacopeia (USP) method, and it was found to be valid for glimepiride within concentration ranges 40 to 140 μg/mL, using C18 analytical columns, and isocratic elution with UV detection, and at 1 mL/min of flow rate.

Development and Validation of an HPLC Method for the Determination of the macrolide antibiotic Clarithromycin using Evaporative Light Scattering Detector in raw materials and Pharmaceutical Formulations

Mediterranean Journal of Chemistry ◽

10.13171/mjc64/01706211420-tzouganaki ◽

2017 ◽

Vol 6 (4) ◽

pp. 133-141 ◽

Cited By ~ 3

Author(s):

Zampia Tzouganaki ◽

Michael Koupparis

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Gas Flow ◽

Raw Materials ◽

Pharmaceutical Formulations ◽

Reversed Phase ◽

Hplc Method ◽

Ich Guidelines ◽

In this work, ELS-Detector has been used for the development of an HPLC method for the determination of clarithromycin in pharmaceutical formulations (tablets and pediatric suspension). Isocratic reversed phase HPLC approach has been developed using a C-18 column (Waters Spherisorb 5 μm ODS2, 4.6x250 mm) and a mobile phase consisting of acetonitrile / aqueous trifluoroacetic acid as pairing reagent. Experimental parameters (temperature of heated drift tube, flow rate of mobile phase, gas flow rate, mobile phase composition) were optimized. Clarithromycin’ s stability was thoroughly examined in different solvent systems. Using the optimized conditions the working range was 5-100 μg/mL (upper limit can be increased considerably), with a detection limit of 4.5 μg/mL (6x10-6 M). The method was validated as per ICH guidelines. The retention time was 4.7 min. The method was successfully applied for the content assay of clarithromycin formulations.