A Thorough HPLC Assay of Quaternary Veterinary Formulation coupled with Environmental Assessment Tool

2021 ◽  
Author(s):  
Adel M Michael ◽  
Yasmin M Fayez ◽  
Hany H Monir ◽  
Christine K Nessim
Keyword(s):  
Environmental Assessment ◽  
Assessment Tool ◽  
Health And Safety ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Hplc Assay ◽  
Vitamin K3 ◽  
Environmental Health And Safety ◽  
Significant Difference

Abstract A new and accurate reversed phase HPLC method with UV detection has been established for any veterinarian analyst for simultaneous determination of a veterinary quaternary mixture of sulphadimidine sodium (SDS), sulphaquinoxaline sodium (SQS), diaveridine (DVD) and vitamin K3 (VTK3) in their formulation. The stationary phase was SEA C18 column (250 × 4.6 mm i.d., 5 μm particle size) at 25°C with an isocratic mode, using a mobile phase containing a mixture of methanol:acetonitrile:distilled water in the ratio of (20:20:60, by volume). The flow rate was 0.8 mL min−1, and UV detection was performed at 230 nm. The HPLC assay was coupled with Environmental Assessment Tool (EAT), which represents a simple and proficient approach for profiling the greenness of the method. This takes into consideration the environmental, health and safety issues for all solvents that involved in the chromatographic method and calculates a total score that can be used for comparison of the greenness of different methods. The method was found to be linear over (0.5–30) μg/mL for all cited drugs with mean percentage recoveries (99.56 ± 1.141) for VTK3, (99.56 ± 1.056) for DVD, (99.62 ± 1.482) for SDS and (99.52 ± 1.205) for SQS. The results were statistically compared with those of the official and reported methods; using Student’s t-test and F-test, showing no significant difference with respect to accuracy. Specificity of the applied method was assessed by analyzing the laboratory-prepared mixtures. The developed method was validated according to ICH guidelines. The proposed methodology can be applied for rapid routine assay of this combination.

scholarly journals Optimization and validation of a new chromatographic method for the assay of veterinary formulation

2019 ◽  
Vol 10 (3) ◽  
pp. 218-223
Author(s):  
Hany Hunter Monir ◽  
Adel Magdy Michael ◽  
Christine Kamal Nessim ◽  
Yasmin Mohamed Fayez ◽  
Nahla Salah Elshater
Keyword(s):  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Fixed Dose ◽  
Selective Determination ◽  
Ich Guidelines ◽  
Significant Difference ◽  
Dose Combination ◽  
Student’S T

New, validated and accurate reversed phase HPLC method with UV detection has been established for simultaneous determination of a veterinary binary mixture of doxycycline hydrochloride (DOX) and tylosin tartrate (TYT). The stationary phase was ACE- 126-2546 AQ C-18 (250 × 4.6 mm i.d., 5 μm particle size) column at 25 °C, in an isocratic mode, using mobile phase containing a mixture of methanol: acetonitrile: distilled water in the ratio of 60:20:20 (v:v:v), with 0.01% trichloroacetic acid at the flow rate of 0.8 mL/min and UV detection was performed at 270 nm. The retention times were 4.02±0.01 and 5.62±0.01 mins for DOX and TYT, respectively. Selective determination of the cited veterinary drugs has been developed in their formulation. The method was found to be linear over 1-50 µg/mL for DOX and TYT with mean percentage recoveries 99.62±1.220 and 100.09±1.104%. The method was proven to be accurate, precise and specific. The obtained results were statistically compared with those of the official and reported methods; using Student’s t test, F test and one-way ANOVA, showing no significant difference with high accuracy. Specificity of the applied method was assessed by analysing the laboratory-prepared mixtures and their combined dosage form. The developed method was confirmed according to ICH guidelines. The validated method can be considered as alternative and basic method for the routine determination of this fixed dose combination with minimum sample preparation.

New and validated RP-HPLC Method for Quantification of Safinamide Mesylate in Presence of Its Basic Degradate, Levodopa and Ondansetron: Application to Human Plasma

2020 ◽  
Vol 58 (9) ◽  
pp. 789-795
Author(s):  
Amira M El-Kosasy ◽  
Lobna A Hussein ◽  
Nesma M Mohamed ◽  
Nahla N Salama
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Pharmaceutical Preparation ◽  
High Sensitivity ◽  
Reversed Phase ◽  
Hplc Method ◽  
Assay Method ◽  
Ultraviolet Detector ◽  
Rp Hplc ◽  
Significant Difference

Abstract A simple, precise, rapid and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for analysis of safinamide mesylate (SAF) in presence of its basic degradate, and co-administered drugs levodopa and ondansetron. The mobile phase consisted of acetonitrile and 20 mM potassium dihyrogen orthophosphate buffer having pH = 5 (40: 60 v/v). Quantification was achieved with ultraviolet detector at 226 nm. The linear range was 0.5–10 μg/mL with mean recovery ± SD of 99.72 ± 1.59. The peak purity of SAF in pharmaceutical preparation spiked with its degradate and co-administered drugs revealed symmetry factor (999.8) within the calculated threshold (>998.1). The suggested method was validated in compliance with the International Conference on Harmonization (ICH) guidelines and statistically compared with the manufacturer HPLC method with no significant difference in terms of accuracy and precision. The assay method was successfully used to estimate SAF in tablets with good percentage recoveries. The high sensitivity (lower than Cmax of the drug 0.65 μg/mL) of the proposed HPLC method enabled the determination of SAF in presence of its basic degradate and co-administered drug, ondansetron in human plasma with acceptable accuracy. The suggested HPLC method could be used in Quality Control (QC) lab for analysis of the studied drug in pharmaceutical preparation.

scholarly journals Chemical Fingerprinting of Hoodia Species and Related Genera: Chemical Analysis of Oxypregnane Glycosides Using High-Performance Liquid Chromatography with UV Detection in Hoodia gordonii

2007 ◽  
Vol 90 (6) ◽  
pp. 1526-1531 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Rahul S Pawar ◽  
Yatin J Shukla ◽  
Ikhlas A Khan
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Hoodia Gordonii ◽  
Succulent Plant ◽  
Hplc Profiles ◽  
Chemical Fingerprinting ◽  
Liquid Chromatographic

Abstract Hoodia gordonii, family Asclepiadaceae, is a succulent plant and is traditionally used in southern Africa for its appetite-suppressant properties. A high-performance liquid chromatographic (HPLC) method with UV detection for analysis of 11 oxypregnane glycosides from H. gordonii has been developed. The simultaneous analysis of 11 oxypregnane glycosides was achieved with a Phenomenex (Torrance, CA) reversed-phase C18 column using gradient mobile phase of water and acetonitrile, both containing 0.025 trifluoroacetic acid. The developed method was applied to the identification of oxypregnane glycosides in 3 different species of Hoodia and 23 related genera. The HPLC profiles of various plant samples were compared for the presence of oxypregnane glycosides.

Molecular and Quantum Mechanical Study for the Separation of Cefprozil in the Presence of Its Alkaline Degradation Product Using RP-HPLC with UV Detection

2017 ◽  
Vol 100 (2) ◽  
pp. 392-399 ◽  
Author(s):  
Khalid A M Attia ◽  
Mohammed W I Nassar ◽  
Mohamed B El-Zeiny ◽  
Ahmed Serag
Keyword(s):  
Degradation Product ◽  
Generation Cephalosporin ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Quantum Mechanical ◽  
Rp Hplc ◽  
Quantum Mechanical Study ◽  
Alkaline Conditions

Abstract A reversed-phase HPLC method (RP-HPLC) with UV detection was developed and validated for the quantitative determination of cefprozil, a second-generation cephalosporin. Due to β-lactam ring instability under alkaline conditions, this RP-HPLC method was applied for the determination of cefprozil in the presence of its possible degradation product. The interactions that govern the separation process with stationary phase were investigated at both molecular and quantum mechanical levels. Moreover, electrostatic potential maps were generated to determine the sites of interaction with mobile phase. The suggested method was validated in compliance with International Conference on Harmonization guidelines and successfully applied for the determination of cefprozil in its commercial pharmaceutical formulation.

Automated HPLC assay of fluoxetine and norfluoxetine in serum

1994 ◽  
Vol 40 (7) ◽  
pp. 1312-1316 ◽  
Author(s):  
J H Nichols ◽  
J R Charlson ◽  
G M Lawson
Keyword(s):  
Solid Phase ◽  
Internal Standard ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hplc Assay ◽  
Spectrophotometric Detection ◽  
Automated Assay ◽  
Automated Method ◽  
Automated Hplc ◽  
Interference Study

Abstract This automated assay determines the concentration of the antidepressant fluoxetine (Prozac) and its active metabolite norfluoxetine in serum by reversed-phase HPLC with spectrophotometric detection. Extraction, injection, and quantification are performed by the Gilson Aspec automated sample handler. The patient's specimen, with added protriptyline as internal standard, is extracted with solid-phase and liquid-liquid methods. Separation is conducted isocratically on a 5-microns (particle size) Supelcosil LC-8-DB reversed-phase column with a triethylamine acetate:acetonitrile mobile phase. The detection limit is 10 micrograms/L and absorbance varies linearly with concentration between 20 and 1,000 micrograms/L for both compounds. Mean recovery was 62% for fluoxetine and 70% for norfluoxetine over linear limits. Within-run and day-to-day imprecision (CV), evaluated at three concentrations (50, 200, and 500 micrograms/L), ranged from 2% to 7%. An extensive interference study of 108 drugs was conducted. Results (n = 58) by the automated method (y) correlated well with those by a manual HPLC method (x): y = 0.96x + 10.20 (r = 0.951, Sylx = 42.9) for fluoxetine, and y = 0.95x - 1.37 (r = 0.917, Sylx = 47.2) for norfluoxetine.

scholarly journals Development of Stability Indicating LC Method for the Estimation of Tolperisone in Bulk and Pharmaceutical Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
U. K. Chhalotiya ◽  
K. K. Bhatt ◽  
D. A. Shah ◽  
S. L. Baldania ◽  
S. B. Patel
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Chemical Oxidation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference ◽  
Alkali Hydrolysis

A rapid, specific, and sensitive reverse phase high performance liquid chromatographic method has been developed and validated for analysis of tolperisone in both bulk and pharmaceutical dosage form. The HPLC method was performed with a reversed phase C18 SunFire column (250 mm × 4.6 mm i.d., 5 mm particle size), detection at 261 nm and a mixture of methanol, water and pH 7.5 adjusted by use of 1% solution of triethylamine (60 : 40) as mobile phase. The flow rate was 1.0 mL min−1 and effluents were monitored at 261 nm. The retention time of tolperisone was 4.8 min. Tolperisone was subjected to acid and alkali hydrolysis, chemical oxidation, wet hydrolysis, dry heat degradation, and sunlight degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. Stressed samples were assayed using developed LC method. The proposed method was validated with respect to linearity, accuracy, precision, and robustness. The method was successfully applied to the estimation of tolperisone in tablet dosage forms.

Simultaneous Determination of Ursodeoxycholic Acid and Chenodeoxycholic Acid in Pharmaceutical Dosage Form by HPLC–UV Detection

2017 ◽  
Vol 100 (1) ◽  
pp. 59-64 ◽  
Author(s):  
Mostafa A Khairy ◽  
Fotouh R Mansour
Keyword(s):  
Ursodeoxycholic Acid ◽  
Simultaneous Determination ◽  
Chenodeoxycholic Acid ◽  
Dosage Form ◽  
Reference Method ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmaceutical Dosage Form

Abstract A reversed-phase HPLC method was developed for the simultaneous determination of ursodeoxycholic acid (UDCA) and the epimeric isomer, chenodeoxycholic acid (CDCA), in their synthetic mixtures and in tablet dosage form. The proposed HPLC method uses a C18 column and mobile phase consisting of an acetonitrile–phosphate buffer mixture (pH 2.3, 100 mM; 50 + 50, v/v) at a flow rate of 2.0 mL/min with UV detection at 210 nm. The method was validated according to the International Conference on Harmonization guidelines; and linearity, range,accuracy, precision, robustness,and system suitability were studied. The LOD and LOQ were also calculated and found to be 1.23 and 3.73 μg/mL for UDCA and 0.83 and 2.52 μg/mL for CDCA, respectively. The method was adapted for UHPLC, in which baseline separation was achieved in <2.5 min. The assay results of Ursomix tablets by the developed method were statistically compared with those obtained by the reference method using t- and F-tests, and no significant differences were observed.

scholarly journals RP-HPLC method with indirect UV detection for determination of sodium ibandronate in pharmaceuticals

2019 ◽  
Vol 64 (02) ◽  
pp. 43-49
Author(s):  
Zharko Tanturovski ◽  
Zorica Arsova-Sarafinovska ◽  
Aneta Dimitrovska
Keyword(s):  
Sodium Salt ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Array Detector ◽  
Ibandronic Acid ◽  
Indirect Uv Detection ◽  
Rp Hplc

Ibandronate sodium (IBN) [(1-hydroxy-3- (methyl pentyl amino) propylidene bisphosphonic acid monosodium monohydrate)] is the sodium salt of ibandronic acid, a synthetic nitrogen-containing bisphosphonate drug. The aim of this study was to develop a sensitive and accurate RP-HPLC method with indirect UV detection for determination of IBN in pharmaceutical formulations. Chromatographic separation was performed on a Waters Bridge C18 reversed-phase column (250 x 4.6 mm I.D.; particle size 5 µm), in an isocratic mode with a mobile phase constituted of 90% buffer: 10% acetonitrile (V/V). The buffer was made using 1.5 mL ortho-phosphoric acid, 990 mg 1-Hexanesulfonic acid sodium salt 98%, 140 mg EDTA in 1000 mL flask diluted with HPLC grade water. The elution was carried out at a flow rate of 1.0 mL minˉ1. A diode array detector measured the UV absorbance at 198 nm, in inverse mode. The method was validated for specificity/selectivity, linearity, LOD, LOQ, accuracy, precision and robustness according to ICH validation guidelines. The limits of detection and quantification were calculated at 0.0163 µg/mL and 0.0495 µg/mL, respectively. The method was effectively used for determination of IBN from commercial tablets and provided good results without any interference from commonly used excipients. Keywords: RP-HPLC with indirect UV detection, Ibandronate sodium, validation, pharmaceuticals

scholarly journals Spectrophotometric and Column High-Performance Liquid Chromatographic Methods for Simultaneous Estimation of Metoprolol Tartrate and Hydrochlorothiazide in Tablets

2008 ◽  
Vol 91 (5) ◽  
pp. 1045-1050 ◽  
Author(s):  
Gopal Garg ◽  
Shailendra Saraf ◽  
Swarnlata Saraf
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Metoprolol Tartrate ◽  
Significant Difference ◽  
Liquid Chromatographic

Abstract Simple, accurate, economical, and reproducible UV spectrophotometric and column high-performance liquid chromatographic (HPLC) methods were developed for simultaneous estimation of a 2-component drug mixture of metoprolol tartrate and hydrochlorothiazide in combined tablet dosage form. The first method used the simultaneous equation method with 7 mixed standards and the absorption maxima at 223 and 271 nm, respectively, for metoprolol tartrate and hydrochlorothiazide in methanol. Linearity was observed in the concentration ranges of 424 and 216 g/mL for metoprolol tartrate and hydrochlorothiazide, respectively. The developed HPLC method used a reversed-phase C18 column and methanolwater (95 + 5) mobile phase at an ambient temperature of 27 2C and UV detection at 225 nm; the run time was 10 min, and quantification was based on peak area. The injection repeatability and intraday and interday repeatability were calculated. Paracetamol was used as an internal standard for the HPLC method, and linearity was observed in the concentration range of 550 g/mL for metoprolol and 220 g/mL for hydrochlorothiazide. The proposed methods were successfully applied for the determination of metoprolol tartrate and hydrochlorothiazide in bulk powder and dosage form. The results obtained were analyzed statistically, and there was no significant difference between the 2 methods. The validation was performed according to International Conference on Harmonization guidelines.

scholarly journals LC Determination and Stability Assessment of Macrolide Antibiotics Azithromycin and Spiramycin in Bulk and Tablet Samples

2015 ◽  
Vol 47 ◽  
pp. 1-10 ◽  
Author(s):  
A. Mahmoudi
Keyword(s):  
Detection Limit ◽  
Ambient Temperature ◽  
Flow Rate ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Macrolide Antibiotics ◽  
Stability Assessment ◽  
Development And Validation

Development and validation of rapid HPLC method for quantifying macrolide antibiotics azithromycin (AZI) and spiramycin (SPI) in bulk and tablet samples is described. Determination was performed on a reversed phase C18 ODB column (250×4.6 nm I.D) at ambient temperature, and employing a UV-detection set at 210 nm. The mobile phase consists of acetonitrile –2-methyl-2-propanol–hydrogenphosphate buffer, pH 6.2, with 1.8% triethylamine (32:8: up to 100, v/v/v), delivered at a flow-rate of 1.1 mL min-1. The assay is linear in concentration ranges of: 0.004–4.8 and 0.0003–1.2 mg mL−1 for azithromycin and spiramycin, respectively, with detection limit of 0.02% for SPI and 0.03% for AZI. Recovery experiments revealed recovery of 98.51–100.82%. The applicability of this method in stability assessment studies is evaluated.

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