scholarly journals Novel Rapid Validated TLC- Densitometry for the Simultaneous Determination of Three Co-formulated Drugs used for Deep Tooth Inflammation Treatment

2021 ◽  
pp. 34-42
Author(s):  
Mohammad Marouf ◽  
Ghoufran Kawas ◽  
Amir Alhaj Sakur
Keyword(s):  
Simultaneous Determination ◽  
Ternary Mixture ◽  
Low Cost ◽  
Control Analysis ◽  
Ich Guidelines ◽  
Rf Values ◽  
Root Canal System ◽  
Developing System ◽  
Layer Chromatography

A new use of a tertiary antibiotic combination of ciprofloxacin, clindamycin and metronidazole is currently being studied as an intracranial (intracranial) drug in an effort to disinfect the root canal system to revitalize the tooth with dead pulp. It is necessary to developing analytical method for the new drug combination. Herein we developed a rapid validated thin-layer chromatography (TLC)‒densitometric method has been developed for the simultaneous determination of 3 co-formulated drugs used for deep tooth inflammation Treatment. The studied drugs are Ciprofloxacin.HCL (CIP), Clindamycin phosphate (CLI) and Metronidazole(MET). The separation was achieved by using silica gel 60 F254 plates (20*20 cm) as stationary Phase and the developing system of Dichloromethane:n-Hexane:methanol:Ethylamine:Triethylamine (40:20:32:3:5)v/v. Densitometry scanning was performed at 220 nm. The Rf values of CIP, CLI and MET were found to be 0.588, 0.776 and 0.898 respectively. The method was validated as per the International Conference on Harmonization (ICH) guidelines and was successfully applied for the analysis of ternary lab made mixture, containing the cited ternary mixture without interference from excipients. There is no previously published TLC–densitometry method for the determination of the previously mentioned ternary mixture. The suggested method is novel, rapid, accurate, reproducible and of low cost, so; thus, it can be used for quality control analysis of these formulations.

scholarly journals Determination of Amlodipine Besilate and Azilsartan Medoxomil by UHPLC, HPTLC and Spectrophotometric Techniques

2019 ◽  
pp. 1-13
Author(s):  
Marwa Mohammed Soliman ◽  
Manal Kamal Darwish ◽  
Sawsan Abdel-Moneem Abdel-Razeq
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Colored Product ◽  
Developing System ◽  
Layer Chromatography ◽  
Azilsartan Medoxomil ◽  
Yellowish Orange

Aims: To develop methods with complete validation according to ICH guidelines and to be applied for the determination of both drugs in laboratory prepared mixtures and in synthetic tablets. Study Design:  Ultra high performance liquid chromatography (UHPLC), High performance thin layer chromatography (HPTLC) and visible spectrophotometric methods are developed for determination of amlodipine besilate and azilsartan medoxomil in laboratory-prepared mixtures and in synthetic tablets. Methodology: Two techniques have been developed for the simultaneous determination of amlodipine besilate and azilsartan medoxomil in pure form and synthetic tablets. The first was UHPLC in which separation was achieved on a C18 column using 0.1% o-phosphoric acid - acetonitrile - methanol (60:10:30, by volume) as mobile phase with detection at 243nm. The second was HPTLC where separation was performed on silica gel 60 F254 plates using chloroform- tolune-methanol-glacial acetic acid (7: 1.5: 1.5: 0.5 by volume) as a developing system and UV detection at 243nm. In addition, visible- spectrophotometric method was developed for determination of amlodipine besilate in presence of azilsartan medoxomil through formation of yellowish orange colored product after reaction of amlodipine besilate with anisaldehde in acid medium with λmax at 443 nm. Results: UHPLC method was linear over the concentration ranges of 2-20 μg/ mL and 4-40 μg/ mL while HPTLC method was linear over the concentration ranges of 0.2 -4.0 μg/ spot and 0.5-8.0 μg/ spot for amlodipine besilate and azilsartan medoxomil, respectively. The visible spectrophotometric method was found to be valid over the concentration range of 10–80 μg/mL for amlodipine besilate. Conclusion: The proposed three techniques are rapid, accurate and precise, thus can be effectively applied for the routine estimation of both drugs in bulk and in their combined formulations.

scholarly journals Validated thin-layer chromatographic method for alternative and simultaneous determination of two anti-gout agents in their fixed dose combinations

2018 ◽  
Vol 16 (1) ◽  
pp. 496-510 ◽  
Author(s):  
Abdel-Maaboud I. Mohamed ◽  
Mahmoud A. Omar ◽  
Sayed M. Derayea ◽  
Mohamed A. Hammad ◽  
Abobakr A. Mohamed
Keyword(s):  
Thin Layer ◽  
Simultaneous Determination ◽  
Polynomial Regression ◽  
Correlation Coefficients ◽  
Quadratic Model ◽  
Fixed Dose ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Layer Chromatography

AbstractA rapid, simple and sensitive thin-layer chromatography (TLC) spectrodensitometric method was developed for the simultaneous determination of colchicine and probenecid in their binary mixtures. The two drugs were quantitatively separated using silica gel 60 F254 as stationary phase and toluene–ethyl acetate–methanol–ammonia (30:20:20:0.1, v/v/v/v) as mobile phase with UV detection at 248 nm for both drugs and at 354 nm for colchicine alone. Both drugs were efficiently separated with Rf values of 0.33±0.03 and 0.60±0.03 for probenecid and colchicine, respectively. The linearity was found to be 16–320 and 120–2400 (ng/band) with quantitation limits of 17.59 and 225.82 ng/band for colchicine and probenecid, respectively, at 248 nm. At 354 nm, the linearity range of colchicine was found 16–240 ng/band with a quantitation limit of 54.03 ng/band. The experimental determination ranges were greatly extended with lower quantitation limits (15.60 and 116.13 ng/band for colchicine and probenecid, respectively at 248 nm, and 13.20 for colchicine at 354 nm) and correlation coefficients were improved when polynomial regression analysis was used. The quadratic model was found to be the best fit for all responses. The method has been validated according to the International Conference on Harmonization (ICH) guidelines providing good correlation coefficients (0.9997-0.9999) for both drugs, and it has been successfully applied in the determination of both drugs in their commercial dosage form without interference from excipients.

Development and Validation of an Eco-Friendly and Low-Cost Method for the Quantification of Cefepime Hydrochloride in Powder for Injectable Solution Using Infrared (IR) Spectroscopy

2020 ◽  
Vol 16 (4) ◽  
pp. 456-464
Author(s):  
Danilo F. Rodrigues ◽  
Hérida R.N. Salgado
Keyword(s):  
Ir Spectroscopy ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Potassium Bromide ◽  
Pharmaceutical Products ◽  
Injectable Formulation ◽  
Ich Guidelines ◽  
Lactam Ring ◽  
Development And Validation

Background: A simple, eco-friendly and low-cost Infrared (IR) method was developed and validated for the analysis of Cefepime Hydrochloride (CEF) in injectable formulation. Different from some other methods, which employ organic solvents in the analyses, this technique does not use these types of solvents, removing large impacts on the environment and risks to operators. Objective: This study aimed at developing and validating a green analytical method using IR spectroscopy for the determination of CEF in pharmaceutical preparations. Methods: The method was validated according to ICH guidelines and the quantification of CEF was performed in the spectral region absorbed at 1815-1745 cm-1 (stretching of the carbonyl group of β- lactam ring). Results: The validated method showed to be linear (r = 0.9999) in the range of 0.2 to 0.6 mg/pellet of potassium bromide, as well as for the parameters of selectivity, precision, accuracy, robustness and Limits of Detection (LOD) and Quantification (LOQ), being able to quantify the CEF in pharmaceutical preparations. The CEF content obtained by the IR method was 103.86%. Conclusion: Thus, the method developed may be an alternative in the quality control of CEF sample in lyophilized powder for injectable solution, as it presented important characteristics in the determination of the pharmaceutical products, with low analysis time and a decrease in the generation of toxic wastes to the environment.

Two Validated Chromatographic Methods for Determination of Ciprofloxacin HCl, One of its Specified Impurities and Fluocinolone Acetonide in Newly Approved Otic Solution

2021 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Israa A Wahba ◽  
Samah S Saad ◽  
Nesrin K Ramadan
Keyword(s):  
High Performance ◽  
Fluocinolone Acetonide ◽  
Ultraviolet Detection ◽  
Chromatographic Methods ◽  
Bulk Powder ◽  
Developing System ◽  
Layer Chromatography ◽  
Chloroform Methanol ◽  
Linear Regressions

Abstract Two sensitive, selective and precise chromatographic methods have been established for concomitant quantification of ciprofloxacin HCl (CIP), fluocinolone acetonide (FLU) along with ciprofloxacin impurity A (CIP-imp A). The first method was thin-layer chromatography (TLC-densitometry) where separation was accomplished using TLC silica plates 60 G.F254 as a stationary phase and chloroform–methanol–33%ammonia (4.6:4.4:1, by volume) as a developing system. The obtained plates were scanned at 260 nm over concentration ranges of 1.0–40.0, 0.6–20.0 and 1.0–40.0 μg band−1 for CIP, FLU and CIP-imp A, respectively. The second method was based on high-performance liquid chromatography using a Zorbax ODS column (5 μm, 150 × 4.6 mm i.d.) where adequate separation was achieved through a mobile phase composed of phosphate buffer pH 3.6–acetonitrile (45:55, v/v) at flow rate 1.0 mL min−1 with ultraviolet detection at 254 nm. Linear regressions were obtained in the range of 1.0–40.0 μg mL−1 for CIP, 0.6–20.0 μg mL−1 for FLU and 1.0–40.0 μg mL−1 for CIP-imp A. The suggested methods were validated in compliance with the International Conference on Harmonization guidelines and were successfully applied for determination of CIP and FLU in bulk powder and newly marketed otic solution.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.

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