Application of Central Composite Design for screening and Optimization of HPTLC method for simultaneous quantitation of Aprepitant, Dexamethasone and Ondansetron in their synthetic mixtures

2021 ◽  
pp. 5531-5539
Author(s):  
Veena Devi Singh ◽  
Vijay Kumar Singh ◽  
Sanjay J Daharwal
Keyword(s):  
Central Composite Design ◽  
Mobile Phase ◽  
Linear Regression Analysis ◽  
Ternary Mixtures ◽  
Ich Guidelines ◽  
Quality Control Testing ◽  
Rf Values ◽  
Chloroform Methanol ◽  
Central Composite ◽  
Hptlc Method

New HPTLC method was developed and optimized for estimation of Ondansetron (OND), Dexamethasone (DEX) and Aprepitant (APT) in laboratory prepared ternary mixtures by using Central composite design (CCD). The independent variables used for the optimization were the acetone content in mobile phase (%mL), distance of developing solvent (cm) and saturation time (min). HPTLC Separation was performed on Precoated silica gel F254 aluminum plate (10X10 cm, 100μm thickness) with a mobile phase consisting of chloroform: methanol: acetone: ethyl acetate: ammonia (9:4:2:5:0.2 % v/v/v/v). Quantification of OND, APT and DEX were achieved based on a Densitometric analysis over the concentration range of 200-1200 ng/band, 500-1000 ng/band and 1000-2000 ng/band, respectively, at 254nm. The method was yielded dense and well-resolved bands at Rf values of 0.54± 0.02, 0.79±0.02 and 0.23±0.01 for OND, APT and DEX, respectively. The linear regression analysis for the calibration plots produced r2= 0.9997, r2= 0.9998 and r2=0.9997 for OND, APT and DEX, respectively. The method was validated according to the ICH guidelines. The robustness test was determined that the selected factors have an insignificant effect on the responses. The results indicated that the method is suitable for the routine quality control testing of OND, APT and DEX in their bulk form.

DEVELOPMENT OF HPTLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND ORNIDAZOLE IN COMBINED DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 36-43
Author(s):  
N. R Dighade ◽  
◽  
M. D Shende ◽  
A. V Kasture
Keyword(s):  
Quality Control ◽  
High Resolution ◽  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Hptlc Method ◽  
Routine Quality Control

A simple and accurate high performance thin layer chromatographic (HPLTC) method has been developed and validated as per ICH guidelines for estimations of Ciprofloxacin (CP) and Ornidazole (ORN) in combined dosage form. The mobile phase was acetonitrile: toluene: water and triethylamine (5.5:1.8:1.5:1.6 V/V) was found to be best which gave high resolution with Rf 0.16 and 0.84 for ciprofloxacin and ornidazole respectively. The linearity of ciprofloxacin and ornidazole was found to be in the range of 0.4 to 0.8 µg/mL and 0.4 to 0.8 µg/mL, respectively. The coefficient of correlation (r2 ) was found to be greater than 0.989 for both the components by this method. The tablet analyses result (n = 5) were found to be > 100.84 % by HPTLC for both the components. The proposed method was found to be simple, accurate and suitable for routine quality control of marketed formulations containing these drugs.

Validated HPTLC Method for the Estimation of Oxetacaine in Pharmaceutical Formulations

2021 ◽  
pp. 5668-5672
Author(s):  
Kavitha J ◽  
Bonda Vismitha ◽  
Kokilambigai KS ◽  
Seetharaman R ◽  
Lakshmi KS
Keyword(s):  
Mobile Phase ◽  
Glacial Acetic Acid ◽  
Current Method ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Relieve Pain ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Chromatographic Resolution ◽  
Hptlc Method

Oxetacaine is a potent local anesthetics used to relieve pain associated with peptic ulcer. The current method details about a rapid, accurate and precise HPTLC technique for the assessment of Oxetacaine in Pharmaceutical formulation. Chromatographic resolution was carried out on precoated HPTLC plates (Silica gel 60 F254 on Aluminum plate) employing methanol: water: glacial acetic acid (8: 1.8: 0.2 v/v/v) as mobile phase. Densitometric assessment was carried out at 220nm [Camag TLC Scanner III with winCATs software (version – 1.3.4)]. The drug was identified with a Rf value of 0.61. The reliability of the projected method was ascertained by evaluating various validation parameters as per ICH guidelines. The proposed technique can evaluate ten or more formulation units concurrently in a single run and affords a more rapid and cost-effective QC tool for regular analysis of Oxetacaine in pharmaceutical formulations.

scholarly journals Application of TLC-Spectrodensitometric and Chemometric Methods for Determination of Momenta® Cream: A Comparative Study Applied on Ternary Mixture

2021 ◽  
Vol 8 (1) ◽  
Author(s):  
Salem H ◽  
◽  
Omar MA ◽  
Derayea SM ◽  
Khalil AA ◽  
...  
Keyword(s):  
Comparative Study ◽  
Pharmaceutical Preparation ◽  
Ternary Mixtures ◽  
Principle Component Regression ◽  
Ich Guidelines ◽  
Miconazole Nitrate ◽  
Aluminum Plates ◽  
Analytical Approaches ◽  
Chloroform Methanol

A comparative study for the validation and advancement of two analytical approaches applied for the simultaneous determination of Mometasone Furoate (MF), Miconazole Nitrate (MIC) and Gentamicin (GM) formulated in Momenta® cream. The first approach was TLC-spectrodensitometric method, which was advanced by separating the three components on TLC aluminum plates coated with silica gel 60 F254 using chloroform: methanol: formic acid (4:0.3:0.15, v/v/v) as a mobile phase, then scanned at 254nm using Camage TLC scanner 3 operated in reflectance-absorbance mode. The second approach was the chemometric method using two models: Partial Least Squares (PLS) and Principle Component Regression Model (PCR). The proposed approaches were validated according to ICH guidelines and were applied for the determination of the ternary mixtures in their analytical mixtures and pharmaceutical preparation.

HIGH-PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR THE SIMULTANEOUS QUANTITATION OF LOPINAVIR AND RITONAVIR IN TABLET FORMULATION

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (01) ◽  
pp. 23-29
Author(s):  
J. D. Fegade ◽  
◽  
N. D Chawla ◽  
R. Y. Chaudhari ◽  
V. R. Patil
Keyword(s):  
Acetic Acid ◽  
High Performance ◽  
Chromatographic Method ◽  
Glacial Acetic Acid ◽  
Solvent System ◽  
Tablet Formulation ◽  
Ich Guidelines ◽  
Rf Values ◽  
Aluminum Plates ◽  
Hptlc Method

The present work describes a simple, accurate and precise HPTLC method for simultaneous quantitation of ritonavir (RVR) and lopinavir (LVR) in tablet formulation. Chromatographic separation of both drugs was performed on precoated aluminum plates, silica gel 60 F254 as the stationary phase and the solvent system consisted of toluene: ethyl acetate: methanol: glacial acetic acid in the ratio of 6.5:2.5:0.5:0.5(v/v/v/v). Densitometric evaluation of the separated zones was performed at 266 nm. The two drugs were satisfactorily resolved with Rf values of 0.242 0.03 and 0.413 0.02 for RVR and LVR, respectively. The accuracy and reliability of the method was assessed by evaluation of linearity (400-2000 ng/spot for RVR and 1600-8000 ng/spot for LVR), precision (intra-day RSD 0.16-0.38% and inter-day RSD 0.21-0.60 % for RVR and intra-day RSD 0.35-0.58 % and inter-day RSD 0.26-0.55 % for LVR) and recovery (99.54 0.62 % for RVR and 100.45 0.65 % for LVR), in accordance with ICH guidelines.

scholarly journals Validated TLC-densitometry method for determination of cetirizine dihydrochloride in tablet dosage form

2013 ◽  
Vol 3 (1) ◽  
pp. 208-210
Author(s):  
Nia Kristiningrum ◽  
Ellsy Novita Martyanti
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
Limit Of Quantification ◽  
Quality Control Testing ◽  
Relative Standard ◽  
Tablet Formulations ◽  
Tablet Dosage ◽  
Chloroform Methanol

A rapid, reproducible and accurate TLC method was developed for the determination of Cetirizine Dihydrochloride in tablet. The analytes were dissolved with ethanol 70% and chromatographed on silica Gel GF 254 TLC plate using chloroform : methanol : ethyl acetate in the ratio of 2 : 7 : 3 (v/v) as mobile phase. Quantitative analysis was done through densitometric measurement at wavelength 234 nm. Method was found linear over the concentration range of 400 – 1600 ng/spot with the correlation coefficient of 0.996. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 75.54 and 226.64 ng/spot. The relative standard deviation of this method was 0.86% whereas the means of the recovery data was 100.54 ± 0.11%. The proposed method has been applied to the determination of Cetirizine Dihydrochloride in commercial tablet formulations and the result were 96.97 ± 0.86 % for brand A and 100.57 ± 1.17 % for brand B. The developed method was successfully used for the assay of Cetirizine Dihydrochloride. This method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v3i1.17294 International Current Pharmaceutical Journal, December 2013, 3(1): 208-210

scholarly journals CENTRAL COMPOSITE DESIGN APPLIED IN HPLC OPTIMIZATION FOR ANALYSIS OF TARTRAZINE AND AURAMINE O IN POWDER DRINKS

2019 ◽  
pp. 211-215
Author(s):  
ANNISA DYAH LESTARI ◽  
Abdul Rohman ◽  
SUDIBYO MARTONO
Keyword(s):  
Central Composite Design ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Acetate Buffer ◽  
Ammonium Acetate Buffer ◽  
Acetate Concentration ◽  
Rp Hplc ◽  
Central Composite

Objective: This study was intended to optimize reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of Tartrazine (TAR) and Auramin O (AUO) in powder drinks using experimental design of central composite design (CCD) approach. Methods: TAR and AUO in powder drink product has same properties, therefore both analytes were analysed using C18 column (XBridge Shield RP 18 250 mm x 4.6 mm i.d., 5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. Some factors responsible for RP-HPLC separation of TAR and AUO including the concentration of buffer, the ratio of mobile phase and flow rate were optimized using CCD. The responses evaluated were peak area, retention time, and tailing factor. The mobile phase used was acetonitrile and ammonium acetate buffer, and acetonitrile composition was optimized at 84-86% for separation of TAR and AUO, delivered at a flow rate of 0.8–1.2 ml/min, using ammonium acetate buffer at 19-21 mmol. Results: CCD showed that separation of TAR and AUO was influenced by flow rate, the ratio of acetonitrile and ammonium acetate concentration. These factors affected significantly to retention time, peak area, and tailing factor. The optimal condition obtained based on CCD was flow rate of 1.2 ml/min, the ratio of acetonitrile 86%, and ammonium acetate concentration of 19 mmol. Conclusion: CCD can be used to get optimum condition for analysis of TAR and AUO in powder drink product.

VALIDATED HPTLC METHOD FOR SIMULTANEOUS DETERMINATION OF OLMESARTAN MEDOXIMIL AND METOPROLOL SUCCINATE IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (10) ◽  
pp. 13-17
Author(s):  
V. V Kunjir ◽  
◽  
S. B. Jadhav ◽  
A. J Purkar ◽  
P. D. Chaudhari
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Metoprolol Succinate ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Hptlc Method

A high performance thin layer chromatographic method has been developed for the simultaneous determination of olmesartan medoximil and metoprolol succinate from tablet dosage form. The mobile phase consisting of water-methanol-ammonium sulphate (4.5:4.5:1.5 v/v/v) and wavelength of detection 233 nm was used. The developed method was validated as per ICH guidelines.

scholarly journals Formulation and Optimization of Carbamazepine Microspheres by 2 Factor 2 Level Central Composite Design

2016 ◽  
Vol 19 (2) ◽  
pp. 152-160 ◽  
Author(s):  
Nusrat Ahmed ◽  
Ikramul Hasan ◽  
Mohammad Saifuddin ◽  
Jakir Ahmed Chowdhury ◽  
Md Selim Reza
Keyword(s):  
Drug Release ◽  
Central Composite Design ◽  
Drug Loading ◽  
Statistical Significance ◽  
Linear Regression Analysis ◽  
Dissolution Time ◽  
Permeability Characteristics ◽  
Optimum Formulation ◽  
Eudragit Rl ◽  
Central Composite

The present investigation was designed to prepare controlled release microspheres of carbamazepine using two polymers of different solubility and permeability characteristics, Ethocel standard 45 premium and Eudragit RL 100. The drug release profile was optimized with the aid of design of experiments (DoE). Microspheres of combined polymers were designed according to 22 factorial central composite design (CCD), taking drug loading and polymeric ratio as the independent variables. Total thirteen batches were prepared. The dependent variables were percentage of drug released in 3 hours and 6 hours and mean dissolution time (MDT). The regression parameters of the developed model and graphical interpretation for each response with statistical significance were calculated by using Minitab 17. The relationship between the experimental variables and responses were evaluated by generating response surface plots. Increased amount of Eudragit RL 100 had impact on surface morphology of prepared microspheres. It produced larger holes on the surface due to its higher permeability characteristics. Polynomial mathematical models generated for various response variables using multiple linear regression analysis, were found to be statistically significant (p < 0.05). One optimum formulation (O1) was selected based on USP specification and the second optimum formulation (O2) was selected for the maximization of MDT (hours). Batch O1 showed 22.85 % and 48.78 % drug release after 3 and 6 hours, respectively which were found to be in close agreement with those predicted by the mathematical model. Another optimum formulation, batch O2 showed MDT as 160.61 hours.Bangladesh Pharmaceutical Journal 19(2): 152-160, 2016

scholarly journals HPTLC-Densitometric Analysis of Eperisone Hydrochloride and Paracetamol in Their Combined Tablet Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nirav Uchadadiya ◽  
Falgun Mehta ◽  
Pinak Sanchaniya
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Glacial Acetic Acid ◽  
Average Recovery ◽  
Form Identification ◽  
Ich Guidelines ◽  
Phase Calibration ◽  
Response Peak ◽  
Tablet Dosage ◽  
Hptlc Method

A simple, precise, accurate, and reliable HPTLC method has been developed and validated for the analysis of EPE-Eperisone hydrochloride and PCM-Paracetamol in their combined dosage form. Identification and analysis were performed on 100 mm × 100 mm layer thickness 0.2 mm, precoated silica gel G60-F254 aluminum sheet, prewashed with methanol, and dried in an oven at 50°C for 5 min. Toluene : methanol : ethyl acetate : glacial acetic acid (4 : 3.5 : 2.5 : 0.05) (v/v/v/v) was used as mobile phase. Calibration plots were established showing the dependence of response (peak area) on the amount chromatographed. The validated calibration ranges were 200–700 ng/spot and 1300–4550 ng/spot for EPE and PCM with correlation coefficient (R2) 0.994 and 0.996, respectively. Average % recovery was between 98.61–100.94% and 99.18–100.57% for EPE and PCM, respectively. The spots were scanned at 248 nm in a reflectance mode. The proposed method was validated as per ICH guidelines and successfully applied to the estimation of EPE and PCM in their combined tablet dosage form.

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