scholarly journals Quantitative Analysis of the Cholesterol-Lowering Drugs Ezetimibe and Simvastatin in Pure Powder, Binary Mixtures, and a Combined Dosage Form by Spectrophotometry, Chemometry, and High-Performance Column Liquid Chromatography

2010 ◽  
Vol 93 (6) ◽  
pp. 1844-1855 ◽  
Author(s):  
Hayam Mahmoud Lotfy ◽  
Amal Mahmoud Aboul Alamein ◽  
Maha Abdel Monem Hegazy
Keyword(s):  
Least Squares ◽  
High Performance ◽  
Dosage Form ◽  
Least Squares Method ◽  
Hplc Method ◽  
Isosbestic Point ◽  
Prediction Ability ◽  
Spectrophotometric Methods ◽  
Significant Difference

Abstract Simple, accurate, sensitive, and precise UV spectrophotometric, chemometric, and HPLC methods were developed for simultaneous determination of a two-component drug mixture of ezetimibe (EZ) and simvastatin (SM) in laboratory-prepared mixtures and a combined tablet dosage form. Four spectrophotometric methods were developed, namely, ratio spectra derivative, ratio subtraction, isosbestic point, and mean centering of ratio spectra. The developed chemometric-assisted spectrophotometric method was the concentration residual augmented classical least-squares method; its prediction ability was assessed and compared to the conventional partial least-squares method. The developed HPLC method used an RP ZORBAX C18 column (5 m particle size, 250 4.6 mm id) with isocratic elution. The mobile phase was acetonitrilepH 3.5 phosphate buffer (40 60, v/v) at a flow rate of 1.0 mL/min, with UV detection at 230 nm. The accuracy, precision, and linearity ranges of the developed methods were determined. The developed methods were successfully applied for determination of EZ and SM in bulk powder, laboratory-prepared mixtures, and a combined dosage form. The results obtained were compared statistically with each other and to those of a reported HPLC method; there was no significant difference between the proposed methods and the reported method regarding both accuracy and precision.

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.

Spectrophotometric Methods for Simultaneous Determination of Sofosbuvir and Ledipasvir (HARVONI Tablet): Comparative Study with Two Generic Products

2017 ◽  
Vol 100 (4) ◽  
pp. 976-984 ◽  
Author(s):  
Nisreen F Abo-Talib ◽  
Mohamed R El-Ghobashy ◽  
Marwa H Tammam
Keyword(s):  
Dosage Form ◽  
Drug Dosage ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Drug Dosage Form ◽  
Generic Products ◽  
Third Derivative ◽  
Combination Pill

Abstract Sofosbuvir and ledipasvir are the first drugs in a combination pill to treat chronic hepatitis C virus. Simple, sensitive, and rapid spectrophotometric methods are presented for the determination of sofosbuvir and ledipasvir in their combined dosage form. These methods were based on direct measurement of ledipasvir at 333 nm (due to the lack of interference of sofosbuvir) over a concentration range of 4.0–14.0 µg/mL, with a mean recovery of 100.78 ± 0.64%. Sofosbuvir was determined, without prior separation, by third-derivative values at 281 nm; derivative ratio values at 265.8 nm utilizing 5.0 µg/mL ledipasvir as a divisor; the ratio difference method using values at 270 and 250 nm using 5.0 µg/mL ledipasvir as a divisor; and the ratio subtraction method using values at 261 nm. These methods were found to be linear for sofosbuvir over a concentration range of 5.0–35.0 µg/mL. The suggested methods were validated according to International Conference on Harmonization guidelines. Statistical analysis of the results showed no significant difference between the proposed methods and the manufacturer's LC method of determination with respect to accuracy and precision. These methods were used to compare the equivalence of an innovator drug dosage form and two generic drug dosage forms of the same strength.

scholarly journals Development and Validation of RP-HPLC Method for the Simultaneous Determination of Rabeprazole Sodium and Itopride Hydrochloride in Solid Dosage Form

2010 ◽  
Vol 7 (3) ◽  
pp. 947-952 ◽  
Author(s):  
Rajesh Sharma ◽  
Ganesh Prasad Mishra ◽  
Subhash Chandra Chaturvedi
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Solid Dosage Form ◽  
Solid Dosage ◽  
Rabeprazole Sodium ◽  
Itopride Hydrochloride

A simple, sensitive, precise, accurate, rapid and reproducible reverse phase high performance liquid chromatographic procedure is developed for simultaneous determination of rabeprazole sodium and itopride hydrochloride in solid dosage form. The mobile phase used was a combination of acetonitrile: buffer (35:65 v/v) and the pH was adjusted to 7.0 ± 0.1 by addition of triethylamine. The detection of the capsule dosage form was carried out at 266 nm and a flow rate employed was 1 mL/min. Linearity was obtained in the concentration range of 2 to 16 μg/mL of rabeprazole sodium and 5 to 55 μg/mL of itopride hydrochloride with a correlation coefficient of 0.9992 and 0.9996 respectively. The results of the analysis were validated statistically and recovery studies confirmed the accuracy of the proposed method.

scholarly journals Determination of Carbamazepine and Its Impurities Iminostilbene and Iminodibenzyl in Solid Dosage Form by Column High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (4) ◽  
pp. 1059-1068 ◽  
Author(s):  
Predrag Lj Džodić ◽  
Ljiljana J ivanovi ◽  
Ana D Proti ◽  
Mira L Zeevi ◽  
Biljana M Joci
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Solid Dosage ◽  
Rp Hplc ◽  
Good Repeatability ◽  
Chemometric Approach

Abstract An accurate and precise RP-HPLC method was developed and validated for the determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in a tablet formulation with fluphenazine as an internal standard. Buffermethanol (50 + 50, v/v) was used as the mobile phase. During validation, specificity, linearity, precision, accuracy, LOD, LOQ, and robustness of the method were tested. The method was proven to be specific against placebo interference. Linearity was evaluated over the concentration range of 100500, 0.050.25, and 0.10.5 g/mL, and the r values were 0.9994, 0.9997, and 0.9979 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Intraday precision of the method was good, and RSD was below 2 for all analytes. The accuracy of the method ranged from 100.69 to 102.10, 99.76 to 102.66, and 99.26 to 100.08 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. LOD was 0.0125, 0.025, and 0.05 g/mL and LOQ was 0.05, 0.05, and 0.1 g/mL for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Robustness of the method was proven by using a chemometric approach. The method was successfully applied to the analysis of commercially available carbamazepine tablets and showed good repeatability, with RSD below 2.

Successive Stability Indicating Spectrophotometric Technique for Simultaneous Determination of Quetiapine Fumarate and its Three Major Related Compounds

2020 ◽  
Vol 16 (4) ◽  
pp. 447-455 ◽  
Author(s):  
Christine M. El-Maraghy ◽  
Ekram H. Mohamed
Keyword(s):  
Hplc Method ◽  
Ternary Mixtures ◽  
Isosbestic Point ◽  
Simultaneous Estimation ◽  
Multicomponent Mixtures ◽  
Zero Crossing ◽  
Quetiapine Fumarate ◽  
Significant Difference ◽  
Related Compounds

Background: Quetiapine Fumarate (QTF) is an atypical antipsychotic drug used to treat mental disorders as depression and schizophrenia. The analysis of the dug in the presence of its precursors, degradants and impurities without interference represents a challenge for the analysts. The regulatory requirements recommended by ICH stated that the impurities above or equal to 0.1% must be identified, characterized and determined. The aim of this work was to introduce three smart and selective spectrophotometric methods that could resolve the complete overlapping of QTF drug with its three related compounds; namely lactam (LAC), N-oxide (OXD) and des-ethanol (DES) without prior separation or extraction step. Methods: So far there is no spectrophotometric method reported in the literature for the analysis of QTF drug with its three related compounds without interference. The First derivative zero crossing (1D-ZC), Spectrum subtraction (SS), and Simultaneous derivative ratio (S1DD) are well-developed methods used for determination and resolution of multicomponent mixtures. While Ratio difference isosbestic point method is a new method that needs two isoabsorptive points for its application and was successfully adopted for simultaneous estimation of ternary mixtures. Results: The linearity range was found in the range of (6-50 μg/mL) for Quetiapine fumarate, (6-110 μg/mL) for lactam, (4-28 μg/mL) for N-oxide and (6-32 μg/mL) for Des-ethanol. The method validation was performed according to ICH guidelines. The results were statistically compared with a reported HPLC method and no significant difference was obtained. Conclusion: The presented spectrophotometric technique highlighted the significance of different tools such as normalized spectra and isoabsorptive points, especially when combined together for the determination and resolution of complex quaternary mixtures as that of QTF and its three major impurities. The proposed methods were smart, accurate and sensitive and were able to determine the four components showing sever overlap without prior separation. The proposed methods are rapid, cheap ecofriendly (green method) and didn’t require any sophisticated programs and could be easily adopted for the routine determination of complex multicomponent mixtures with minimum sample preparation.

Simultaneous Estimation of Chlorpheniramine Maleate and Glyceryl Guaiacolate in Pure and Capsule Dosage form by using different Spectrophotometric Methods

2021 ◽  
pp. 2608-2612
Author(s):  
Nada Ghaaeb Hussein ◽  
Ahmed Mahdi Saeed
Keyword(s):  
Dosage Form ◽  
Solvent Mixture ◽  
Isosbestic Point ◽  
Simultaneous Estimation ◽  
Chlorpheniramine Maleate ◽  
Spectrophotometric Methods ◽  
Percentage Recovery ◽  
Acceptable Range ◽  
Antibiotic Drug

Chlorpheniramine Maleate (CPM) and Glyceryl Guaiacolate (GUA) are the β‐lactum antibiotic drug. Sensitive, precise, accurate and simple, UV spectrophotometric methods have been developed for the simultaneous estimation of Chlorpheniramine Maleate (CPM) and Glyceryl Guaiacolate (GUA) in dosage form. Two spectrophotometric methods (simultaneoue equations and Q‐Absorbance ratio) were applied for the determination of the drugs as mixture. The maximum absorbance of drug in solvent mixture composed of water – acetontrile – methanol in a ratio of (80% H2O – 10% ACN – 10% MOH) was found to be at (261.4 nm and 273 nm) for CPM, GUA respectively, and the Q – isosbestic point was found at 270.4 nm. These wavelengths were selected for the analysis of drugs as mixtures standard and in the manufactured samples using the two developed methods. The methods were linear in the range of (1- 100) μg/mL for (CPM, GUA), with an R2 of (0.9996) for CPM and GUA respectively in the mixture. Recovery means were found to be (99.79 % - 100.30 %) for the standard drugs CPM and GUA respectively and in formulating drugs was found to be (99.71 – 100.41 %). LOD and LOQ were established and found to be (0.1 and 0.33) for CPM and GUA respectively. The method was applied for the estimation of the active gradient of the drugs in different samples of manufactured dosage. The accuracy of method was validated by mean percentage recovery, which was found to be in the acceptable range.

scholarly journals A Validated High-Performance Thin-Layer Chromatographic Method for the Simultaneous Determination of Zofenopril Calcium and Hydrochlorothiazide in the Presence of the Hydrochlorothiazide Impurities: Chlorothiazide and Salamide

2018 ◽  
Vol 101 (4) ◽  
pp. 1031-1041 ◽  
Author(s):  
Mamdouh R Rezk ◽  
Ahmed S Fayed ◽  
Hoda M Marzouk ◽  
Samah S Abbas
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Raw Materials ◽  
Drug Product ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Significant Difference ◽  
Hptlc Method

Abstract The chromatographic analysis of either process-related impurities or degradation products is very important in the pharmaceutical industry. In this work, a simple, selective, and sensitive HPTLC method was developed and validated for the simultaneous determination of zofenopril calcium (ZOF) and hydrochlorothiazide (HCT) in the presence of the HCT impurities: A) chlorothiazide (CT) and B) salamide, in raw materials and in pharmaceutical formulation. The separation was carried out on HPTLC silica gel 60 F254 using ethyl acetate–glacial acetic acid–triethylamine (10 + 0.1 + 0.1, v/v/v) as a developing system. The separated bands were scanned densitometrically at 270 nm. Polynomial equations were used for the regression. Calibration curves were constructed for ZOF, HCT, CT, and salamide in the ranges of 0.5–10, 0.2–4, 0.05–1.4, and 0.05–1.0 μg/band, respectively. Different parameters affecting the suggested method, including developing systems of varying composition/ratios and different detection wavelengths, were studied to achieve the best resolution and precision with good sensitivity. System suitability parameters were also tested. The proposed method was validated as per the International Conference on Harmonization guidelines and was successfully applied for the quantification of the studied drugs in their pharmaceutical formulation, with no interference from excipients observed. The results obtained by the developed HPTLC method were compared statistically with those obtained by the reported HPLC method using Student’s t and F ratio tests, and no significant difference was obtained, indicating the ability of the proposed method to be used for routine analysis of drug product.

Partial Least-Squares and Linear Support Vector Regression Chemometric Methods for Simultaneous Determination of Amoxicillin Trihydrate and Dicloxacillin Sodium in the Presence of Their Common Impurity

2016 ◽  
Vol 99 (4) ◽  
pp. 972-979
Author(s):  
Ibrahim A Naguib ◽  
Eglal A Abdelaleem ◽  
Hala E Zaazaa ◽  
Essraa A Hussein
Keyword(s):  
Least Squares ◽  
Support Vector Regression ◽  
Partial Least Squares ◽  
Dosage Form ◽  
Support Vector ◽  
Prediction Ability ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference ◽  
Amoxicillin Trihydrate ◽  
Plsr Model

Abstract Two multivariate chemometric models, namely, partial least-squares regression (PLSR) and linear support vector regression (SVR), are presented for the analysis of amoxicillin trihydrate and dicloxacillin sodium in the presence of their common impurity (6-aminopenicillanic acid) in raw materials and in pharmaceutical dosage form via handling UV spectral data and making a modest comparison between the two models, highlighting the advantages and limitations of each. For optimum analysis, a three-factor, four-level experimental design was established, resulting in a training set of 16 mixtures containing different ratios of interfering species. To validate the prediction ability of the suggested models, an independent test set consisting of eight mixtures was used. The presented results show the ability of the two proposed models to determine the two drugs simultaneously in the presence of small levels of the common impurity with high accuracy and selectivity. The analysis results of the dosage form were statistically compared to a reported HPLC method, with no significant difference regarding accuracy and precision, indicating the ability of the suggested multivariate calibration models to be reliable and suitable for routine analysis of the drug product. Compared to the PLSR model, the SVR model gives more accurate results with a lower prediction error, as well as high generalization ability; however, the PLSR model is easy to handle and fast to optimize.

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