A GC–ECD Method for Analysis of Prasugrel in Bulk and Pharmaceutical Dosage Forms

2015 ◽  
Vol 8 (1) ◽  
pp. 2742-2747
Author(s):  
Samer Housheh ◽  
Saleh Trefi ◽  
Haroun Mohammad ◽  
Fawaz Chehna M
Keyword(s):  
Chromatographic Analysis ◽  
Capillary Column ◽  
Dosage Forms ◽  
Electron Capture Detection ◽  
Optimum Conditions ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Before And After ◽  
Adp Receptor ◽  
Good Retention

Prasugrel is a novel ADP receptor inhibitor with antithrombotic properties. This paper proposes a new method for quantitative analysis of prasugrel in bulk and pharmaceutical dosage forms. The method used gas chromatography with electron-capture detection (GC–ECD). Chromatographic analysis was performed on an RTX-5 capillary column. Under the optimum conditions, good retention and peak response were achieved for prasugrel. The analytical method was fully validated by assessment of LOD and LOQ (0.24 µg/mL and 0.73 µg/mL), linearity (R = 0.997) over the range 0.5-2.5 µg/mL and extraction recovery (>98.7 %, with RSD below 1.0, for prasugrel spiked at 0.5, 1, 1.25, 2 and 2.5 µg/mL), the precision was 0.825% and the intermediate precision was 1.134%. The method required no clean-up of prasugrel before and after injection. It has been successfully used to determine prasugrel content in different commercial pharmaceutical dosage forms.  

SIMULTANEOUS ESTIMATION AND VALIDATION OF RAMIPRIL AND TELMISARTAN BY UV SPECTROPHOTOMETRY

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (09) ◽  
pp. 31-35
Author(s):  
R Rambabu ◽  
◽  
S Vidyadhara ◽  
J Subbarao
Keyword(s):  
Spectrophotometric Method ◽  
Correlation Coefficients ◽  
Simultaneous Equation ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Uv Spectrophotometry ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Sensitive Spectrophotometric Method

A simple and sensitive spectrophotometric method for the determination of ramipril and telmisartan in pharmaceutical dosage forms has been developed. The absorption maxima were found at 220nm for ramipril and 297nm for telmisartan using 0.1N NaOH as solvent. Beer’s law was obeyed for both the drugs in the concentration range of 2-10μg/ml with correlation coefficients 0.999 for both ramipril and telmisartan. The limits of detection for ramipril and telmisartan were found to be 0.142 and 0.405μg/mL respectively and the limits of quantitation were 0.43 and 1.22μg/mL. Accuracy of the method was verified by performing recovery studies using simultaneous equation method and found to be 98.33 to 99.54%w/w for ramipril and 99.36 to 99.82 %w/w for telmisartan. %RSD of repeatability and intermediate precision studies were found to be <2 for both the drugs. Ruggedness of the method was checked by changing analyst worked and instrument used. In both the cases, the %RSD was found to be less than 2.

scholarly journals Utility of N-Bromosuccinimide as a Green Chemical Reagent for Determination of H2-Receptor Antagonists in their Pharmaceutical Dosage Forms

2019 ◽  
Vol 27 (1) ◽  
pp. 47-64
Author(s):  
Ahmed I. Hassan
Keyword(s):  
Correlation Coefficients ◽  
Dosage Forms ◽  
Optimum Conditions ◽  
Linear Calibration ◽  
Receptor Antagonists ◽  
Pharmaceutical Dosage Forms ◽  
Drug Concentrations ◽  
Environmentally Safe ◽  
The Common

Abstract An environmentally safe, simple and robust spectrophotometric method has been developed for determination of H2-receptor antagonists namely: cimetidine (CIM), famotidine (FAM), nizatidine (NIZ), and ranitidine hydrochloride (RAN). The method was depend on the reaction of the studied drugs with N-bromosuccinimide (NBS), environmentally friendly reagent, and the excess NBS was measured by its reaction with phloroglucinol to give a yellow chromogenic product (λmax at 435 nm). The absorption intensity decrease (ΔA) was correlated with drug concentrations in the sample solutions. By using of the optimum conditions, linear calibration curves with good correlation coefficients (0.9958–0.9998) were found between the measured ΔA values and the corresponding drugs concentrations in the range of 12-80 μg mL−1. Limits of detection were in the range 1.31-2.21 μg mL−1. The proposed method was validated and successfully applied for the analysis of the above mentioned drugs in their bulk and pharmaceutical dosage forms with good recoveries (98.5 ± 0.98 to 102.5 ± 0.79%). No interferences were obtained from the common excipients. The proposed method was successfully applied for the analysis of H2RAs in their dosage forms and the results were comparable with that obtained by the official methods.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

scholarly journals Analytical method development and validation of L-Carnitine L-Tartarate in Pharmaceutical Dosage forms (Multivitamin tablets) using non aqueous titration

2019 ◽  
Vol 9 (4) ◽  
pp. 588-590
Author(s):  
Sunil Kumar ◽  
Bigan Ram
Keyword(s):  
Correlation Coefficient ◽  
Analytical Method ◽  
Method Development ◽  
Accurate Method ◽  
Dosage Forms ◽  
Parameter Study ◽  
Titration Method ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Development And Validation

The   Non aqueous titration   method was developed for quantitave analysis of  L-  Carnitine L-Tartarate    in  multivitamin  tablets. The   Non aqueous titration method was carried out using 0.1  N  Perchloric acids. The   present   analytical    method   was validated according to ICH guidelines  (ICH,Q2(R1)).  The   calibration   curve   was  found    to   linear  with correlation coefficient   (r2=0.99995),  Bias   (-0.35)  in  the  range  of  50  to 150  %  of  standard solution. The   precision   and   recovery   were determined   and  all  the  parameter value found within acceptance  limit. The  value  for  both method  and intermediate  precision were found to 0.57 % and recovery  found  to 99.11 to 99.59 %.  The   validation parameter  study  was  method  precision,  intermediate   precision,   Linearity   and   recovery.  This is a   convenient, precise   and   rapid    accurate  method    for  the estimation  of   L-Carnitine  L-Tartarate  in  Bulk  and Pharmaceutical dosage forms (Multivitamin Tablets). Keywords: AIDS, Linearity, Correlation coefficient, Bias, Precision and Recovery

scholarly journals A NOVEL SPECTROPHOTOMETRIC DETERMINATION OF METHYLDOPA THROUGH TERNARY COMPLEXATION PROCEDURE USING FE(III), MN(II), AND CO(II) WITH 2-AMINOPYRIDINE

2019 ◽  
pp. 366-371 ◽  
Author(s):  
MUSTAFA JAMAL KHALEEL BICHAN ◽  
FADAM MUTEB ABDOON
Keyword(s):  
Low Cost ◽  
Dosage Forms ◽  
Optimum Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Ternary Complexation ◽  
Colored Complexes

Objective: The present study is aimed to find a three simple, low cost, accurate, rapid, and sensitive spectrophotometric methods based on the formation of ternary complexes to assay methyldopa (MTD) in both pure and pharmaceutical dosage forms. Methods: The suggested complexation procedure is based on the formation of ternary complex among MTD, 2-aminopyridine (2-Amp), and different metal cations such as [Fe(III), Mn(II), and Co(II)] to form three complexes of Fe(III)-MTD-2-Amp (A), Mn(II)-MTD-2-Amp (B), and Co(II)-MTD-2-Amp (C) in an aqueous medium. Results: The obtained colored complexes are spectrophotometrically measured for the previously mentioned complexes at 572, 473, and 465 nm, respectively. Under optimum conditions, the complexes exhibited apparent, molar absorptivities of 1810.62, 2954.18, and 2596.8 l/mol/cm, Sandell’s sensitivity of 0.132, 0.08, and 0.092 μg/cm2, and Beer–Lambert’s law is obeyed over the ranges 4–40, 4–32, and 4–40 μg/ml for the three developed methods, respectively. Conclusion: The developed spectrophotometric methods showed excellent results in regard to accuracy and precision with recovery of 99.48±1.62%, 100.24±1.76%, and 100.72±1.65% of the complexes A, B, and C, respectively. The obtained results are compared statistically with a reported method with respect to t- and F-tests and the calculated results displayed no significant difference.

scholarly journals Complete Cocrystal Formation during Resonant Acoustic Wet Granulation: Effect of Granulation Liquids

Pharmaceutics ◽  
2021 ◽  
Vol 13 (1) ◽  
pp. 56
Author(s):  
Ryoma Tanaka ◽  
Supisara Osotprasit ◽  
Jomjai Peerapattana ◽  
Kazuhide Ashizawa ◽  
Yusuke Hattori ◽  
...  
Keyword(s):  
Citric Acid ◽  
Fine Powder ◽  
Hydroxypropyl Cellulose ◽  
Dosage Forms ◽  
Wet Granulation ◽  
Unit Operation ◽  
Solid Product ◽  
Pharmaceutical Dosage Forms ◽  
Granulation Process ◽  
Before And After

The manufacturing of solid pharmaceutical dosage forms composed of cocrystals requires numerous processes during which there is risk of dissociation into parent molecules. Resonant acoustic wet granulation (RAG) was devised in an effort to complete theophylline–citric acid (THPCIT) cocrystal formation during the granulation process, thereby reducing the number of operations. In addition, the influence of granulation liquid was investigated. A mixture of anhydrous THP (drug), anhydrous CIT (coformer), and hydroxypropyl cellulose (granulating agent) was processed by RAG with water or ethanol as a granulation liquid. The purposes were to (i) form granules using RAG as a breakthrough method; (ii) accomplish the cocrystallization during the integrated unit operation; and (iii) characterize the final solid product (i.e., tablet). The RAG procedure achieved complete cocrystal formation (>99%) and adequately sized granules (d50: >250 μm). The granulation using water (GW) facilitated formation of cocrystal hydrate which were then transformed into anhydrous cocrystal after drying, while the granulation using ethanol (GE) resulted in the formation of anhydrous cocrystal before and after drying. The dissolution of the highly dense GW tablet, which was compressed from granules including fine powder due to the dehydration, was slower than that of the GE tablet.

Development and Validation of Mebeverine Hydrochloride Assay by RP-HPLC Method

2018 ◽  
Vol 11 (5) ◽  
pp. 4239-4243
Author(s):  
Akbar Syed ◽  
Shaik Haroon Rasheed ◽  
Shaik Afroz ◽  
Syeda Wasfiya Noor ◽  
Syeda Saniya Fatima ◽  
...  
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Chromatographic Peak ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Mebeverine Hydrochloride ◽  
Development And Validation ◽  
Relationship Of

A validated method for the estimation of the mebeverine hydrochloride, an anti-spasmodic agent, was developed which was simple, precise, rapid and accurate. A clear separated chromatographic peak was achieved on Apollo C18 (4.6x250 mm), 5-μm column. Mobile phase used in this separation was the mixture of methanol and water in the ratio of 90:10% v/v with a flow rate of 0.9 μL/min at ambient temperature. The detection was achieved at a wavelength of 265 nm. At the retention time of 3.9 min and tailing factor of 1.09, chromatographic peak was observed. As per the guidelines of ICH, the method was developed and was validated with respect to accuracy, linearity, specificity, precision and robustness. Correlation co-efficient obtained shows a good linear relationship of more than 0.998 in the concentration range of 5 μg to 30 μg. Mean % recovery of 99.2% was seen and %RSD for repeatability and intermediate precision was less than 2%. Therefore, the developed method can be used for the quantitative determination of mebeverine hydrochloride successfully in pharmaceutical dosage forms.

scholarly journals Development and validation of stability indicating RP-HPLC method for the determination of related substances in Raloxifene hydrochloride tablets dosage forms

2019 ◽  
Vol 10 (4) ◽  
pp. 3325-3331
Author(s):  
Babu C ◽  
Suresh Reddy K.V.N ◽  
Shashi Kumar K.N
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Related Substances ◽  
Raloxifene Hcl

This work is intended to thrive a stability-indicating high performance liquid chromatographic method for the analysis of Raloxifene HCl related compounds in pharmaceutical dosage forms. The separation was achieved Inertsil C8 (150 x 4.6 mm ID, 3.5μm)column using a gradient method. Mobile phase A is 0.01M KH2PO4 buffer (pH4.5), and mobile phase B is acetonitrile used in this work. 1.0 mL/ minute is the flow of rate and at 280nm noticed wavelength is monitored. For specificity, the limit of quantification, the limit of detection, linearity, accuracy, method precision, intermediate precision, robustness and stability this method is validated. The six injection impurities of standard solutions at the 4.0 µg/mL conjecture concentration were confirmed experimentally for LOQ values. The correlation coefficient of the impurities is more than 0.99. All impurities meet the criteria for linearity of both the impurities and raloxifene. The RSD recoveries obtained for impurities are not more than 10%. The achievement of this study demonstrated that the method is selective, linear, precise, rugged, robust and stability-indicating for the determination of related substances in raloxifene HCl tablet dosage form.

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