scholarly journals Stability-Indicating RP-HPLC Method for Analysis of Paracetamol and Tramadol in a Pharmaceutical Dosage Form

2012 ◽  
Vol 9 (3) ◽  
pp. 1347-1356 ◽  
Author(s):  
Rajesh M. Kamble ◽  
Shrawan G. Singh
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Water Ph ◽  
The Stability

A simple, isocratic, rapid and accurate reversed phase high performance liquid chromatography method was developed for the quantitative determination of paracetamol and tramadol in commercial medicinal tablets. The chromatographic separation was achieved on an Intersil C18(250 mm x 4.6 mm, 5μm) column using water pH 3.4 with orthophosphoric acid: methanol (60:40, v/v) as a mobile phase, and UV detection at 228 nm. The chromatographic resolutions between paracetamol and tramadol were found greater than five. The linear range for paracetamol and tramadol were 20.8–39.0 μg/ml and 2.4–4.5 μg/ ml was obtained with correlation coefficients ≥0.999 for each analyte. The retention time were found to be 2.1 and 3.9 min for tramadol and paracetamol respectively. Paracetamol and tramadol was subjected to stress conditions (hydrolysis (acid, base) oxidation, photolysis and thermal degradation) and the stressed samples were analyzed by use of the method. The major degradation was observed in acid and minor in base, thermal, oxidation and photolysis. The forced degradation studies prove the stability indicating power of the method.

DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING RP-HPLC METHOD FOR ESTIMATION OF AMBRISENTAN AND ITS PROCESS-RELATED IMPURITIES IN BULK AND PHARMACEUTICAL DOSAGE FORMS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 34-41
Author(s):  
S. K Kondila ◽  
◽  
K Sujana ◽  
A Prameela Rani
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Acid And Base

The aim of the present work was to develop and validate an accurate, precise, simple, and efficient stability indicating Reversed phase High Performance Liquid Chromatography method for determination of an abrisentan and its process impurities in bulk and pharmaceutical dosage forms. The drug substance was subjected to stress conditions such as hydrolysis (acid and base), oxidation, photolysis and thermal degradation as per International Conference on Harmonization guidelines to study the stability-indicating profile of drug. Significant degradation was observed during acid hydrolysis and peroxide degradation. The chromatographic conditions were optimized using an impurity-spiked solution and samples generated from forced degradation studies. The method was developed using Agilent XDB-C18 (150×4.5mm, 5μ) column and 10mM NH4OAc (pH-5.2 adjusted with acetic acid): ACN as the mobile phase with gradient programme at a flow rate of 1 mL/min. effluents were monitored at 289 nm. The retention times were found as 25.945 min for IMP-1, 24.685 min for IMP-2, 23.83 min for IMP-3, 10.53 min for AMB, 5011 min for IMP-4 and 3.48 min for IMP-5. The mean recovery values were found to be 98.52-100.44% for AMD and its impurities. The degradation rate of AMB in acid, base, peroxide (oxidative) thermal and photolytic degradation processes was found in range 7-22%. The developed analytical method has been validated for specificity, linearity, precision, accuracy, and robustness which were within the acceptance limit according to ICH guidelines. The developed method was successfully employed for routine quality control and stability analysis of AMB in pharmaceutical dosage forms.

scholarly journals Development and Validation of a Novel Stability-Indicating Reversed-Phase High-Performance Liquid Chromatography Method for Assay of Loratadine and Determination of Its Related Compounds

2010 ◽  
Vol 93 (3) ◽  
pp. 891-903 ◽  
Author(s):  
Jun Lu ◽  
Yu-Chien Wei ◽  
Robert J Markovich ◽  
Abu M Rustum
Keyword(s):  
High Performance ◽  
Sodium Dodecyl ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Chromatography Method ◽  
Stability Indicating ◽  
The Stability ◽  
Related Compounds

Abstract Loratadine is an important active pharmaceutical ingredient used in a wide variety of prescription and over-the-counter products for the treatment and relief of allergy symptoms. A novel stability-indicating gradient ion-pair RP-HPLC method for assay of loratadine and determination of both of its degradation compounds and process impurities has been developed. This method can separate loratadine from its eight structurally related compounds; it can also separate all of the related compounds from each other in less than 20 min. The stability-indicating capability of this method has been demonstrated by analyzing aged stability samples of loratadine. A 15 cm 4.6 mm id YMC-Pack Pro C18 HPLC column was the primary column and a 15 cm 4.6 mm id SunFire C18 column has been identified as an alternate (truly equivalent) column for this method. This gradient method uses mobile phases consisting of acetonitrile and an aqueous solution of 10 mM sodium acetate and 5 mM sodium dodecyl sulfate at pH 5.5. The new HPLC method was validated according to International Conference on Harmonization guidelines and proved to be suitable for routine QC use.

scholarly journals STABILITY-INDICATING REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS ESTIMATION OF DARUNAVIR AND RITONAVIR

2016 ◽  
pp. 66
Author(s):  
Sindu Priya Dasyam ◽  
Gowri Sankar D ◽  
Masthanamma Sk
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

<p>ABSTRACT<br />Objective: The main objective of the proposed study was to develop and validate a new stability indicating reverse phase high performance liquid<br />chromatography method for the simultaneous estimation of darunavir (DRV) and ritonavir (RTV).<br />Methods: The method was optimized using Atlantis C18 column (50 mm×4.6 mm, 5 µm, Waters Corporation, Milford, USA). Acetonitrile and water<br />were used as mobile phase in the proportion of 60:40. The flow rate was 0.8 ml/minutes and the effluent was monitored at 230 nm.<br />Results: The retention time of DRV and RTV was 3.15 minutes and 4.59 minutes, respectively. The method was precise as it showed a % relative<br />standard deviation of &lt;2%. The percentage recoveries of both the drugs DRV and RTV were 99.8-100.01% and 99.5-99.97%, respectively. The<br />linearity of DRV and RTV was in the range of 40-120 and 4-20 µg/ml, respectively. Calibration curve showed good linearity and range. The correlation<br />coefficient of DRV and RTV was 0.999 each. Moreover, the results obtained for limit of quantification, limit of detection, robustness, and ruggedness<br />were well within the acceptance criteria.<br />Conclusion: The proposed method was found to be simple, rapid, accurate, precise, and stability indicating. It was found to be economical and suitable<br />for simultaneous determination of DRV and RTV which is can also be applied for pharmaceutical dosage form.<br />Keywords: Darunavir, Ritonavir, Reversed-phase-high performance liquid chromatography, Simultaneous estimation, Forced degradation.</p>

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

scholarly journals SIMULTANEOUS ESTIMATION, VALIDATION, AND FORCED DEGRADATION STUDIES OF BETAHISTINE DIHYDROCHLORIDE AND DOMPERIDONE IN A PHARMACEUTICAL DOSAGE FORM USING RP-HPLC METHOD

2018 ◽  
Vol 11 (10) ◽  
pp. 125
Author(s):  
Vaishali Mistry ◽  
Rohan Mishra
Keyword(s):  
Hplc Method ◽  
Base Hydrolysis ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Betahistine Dihydrochloride ◽  
The Stability

Objective: This study describes the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of betahistine dihydrochloride and domperidone in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic operation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 80:20% v/v and eluents were scanned using a UV detector at 244 nm.Results: The retention time of betahistine dihydrochloride and domperidone was found to be 2.3 and 3.6 min, respectively. A linearity response was observed in the concentration range of 9.6 μg/ml–22.4 μg/ml for betahistine dihydrochloride and 6–14 μg/ml for domperidone, respectively. Limit of detection and limit of quantification for betahistine dihydrochloride were 0.52 μg/ml and 1.58 μg/ml and for domperidone are 0.64 μg/ml and 1.94 μg/ml, respectively.Conclusion: The stability-indicating method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

scholarly journals Stability Indicating HPLC Method for Simultaneous Quantification of Trihexyphenidyl Hydrochloride, Trifluoperazine Hydrochloride and Chlorpromazine Hydrochloride from Tablet Formulation

2010 ◽  
Vol 7 (s1) ◽  
pp. S299-S313 ◽  
Author(s):  
P. Shetti ◽  
A. Venkatachalam
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Forced Degradation ◽  
Chlorpromazine Hydrochloride ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Liquid Chromatographic

A new, simple, precise, rapid, selective and stability indicating reversed-phase high performance liquid chromatographic (HPLC) method has been developed and validated for simultaneous quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and chlorpromazine hydrochloride from combined tablet formulation. The method is based on reverse-phase using C-18 (250×4.6) mm, 5 μm particle size column. The separation is achieved using isocratic elution by methanol and ammonium acetate buffer (1% w/v, pH 6.5) in the ratio of 85:15 v/v, pumped at flow rate 1.0 mL/min and UV detection at 215 nm. The column is maintained at 30 °C through out the analysis. This method gives baseline resolution. The total run time is 15 min. Stability indicating capability is established buy forced degradation experiment. The method is validated for specificity, accuracy, precision and linearity as per International conference of harmonisation (ICH). The method is accurate and linear for quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and Chlorpromazine hydrochloride between 5 - 15 μg/mL, 12.5- 37.5 μg/mL and 62.5 - 187.5 μg/mL respectively.

scholarly journals Development and Validation of Stability-Indicating Reverse Phase-High Performance Liquid Chromatography Method for Simultaneous Determination of Atenolol and Nifedipine in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 219-223
Author(s):  
Ansari Yaasir Ahmed ◽  
Qazi Shoeb ◽  
Umme Rumana ◽  
Patel Afroza ◽  
Pathan Vahid Tajkhan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Limit Of Quantitation

The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectively, for NIFE. The method was linear, simple, precise, and accurate and, therefore, suitable for routine analysis of drugs in tablet form. The forced degradation studies were also done through the exposure of analyte solution to four different stress conditions.

scholarly journals A SIMULTANEOUS ESTIMATION, VALIDATION AND FORCED DEGRADATION STUDIES OF 5-FLUOROURACIL AND TEGAFUR IN A PHARMACEUTICAL DOSAGE FORM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2018 ◽  
Vol 11 (12) ◽  
pp. 132
Author(s):  
Vaishali Mistry ◽  
Akshay Yelwe ◽  
Amey Deshpande
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
The Stability

Objective: The present study describes the stability indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of 5-fluorouracil and tegafur in pharmaceutical dosage forms.Method: 5-fluorouracil and tegafur the propose RP-HPLC method were developed by using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic separation was carried on shim-pack gist c18 (250 × 4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 50:50% v/v and elements were scanned using a UV detector at 271 nm.Result: The retention time of 5-fluorouracil and tegafur was found to be 2.74 and 3.66 min, respectively. A linearity response was observed in the concentration range of 13.4 μg/ml–31.3 μg/ml for 5-fluorouracil and 6 μg/ml–14 μg/ml for tegafur, respectively. Limit of detection and limit of quantification of 5-fluorouracil were 10.97 μg/ml and 33.26 μg/ml and for tegafur are 4.89 μg/ml and 14.83 μg/ml, respectively.Conclusion: The stability indicating that the method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

scholarly journals Stability Indicating RP-HPLC for Quantification Mangiferin in Extract of Three Species Mango Leaves

2020 ◽  
Vol 8 (1) ◽  
pp. 15-20
Author(s):  
Yuni Retnaningtyas ◽  
Nia Kristiningrum ◽  
Hidayah Dwi Renggani ◽  
Indah Purnama Sary
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Mangifera Indica ◽  
Reversed Phase ◽  
Hplc Method ◽  
Complete Separation ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Mango Leaves ◽  
The Stability

The stability indication of Reversed Phase-High Performance Liquid Chromatography (RP-HPLC) method was validated for quantitative determination of mangiferin on three species mango leaves (Mangifera odorata Griff, Mangifera foetida Lour, and Mangifera indica L.). The samples were extracted by maseration method using methanol and concentrated using rotary evaporator. The method carried out on stationary phase a purospher RP-18 endcapped (25 cm × 4.6 mm i.d., 5 µm) column with a mobile phase consisting of methanol: phosphoric acid 0.1% (v/v) (31:69); flow rate:0.8 mL/min; solvent methanol, detection was carried out at 258 nm. The analytical  performace this measurement is good with the value of linearity (r2=0.998), precision (%RSD=0.649%), and accuration (10.67%). The forced degradation studies were carried out according to the International Conference on Harmonization (ICH) guidelines. The results indicating that the complete separation between degradation products and mangiferin peak occured. The degradation limit of mangiferin 5–20% (according to the guideline of ICH) except in basic condition (100%). The method was succesful applied to determine of the mangiferin in  pakel (Mangifera foetida), kweni (Mangifera indica) and kopyor (Mangifera odorata) extract. The mangiferin content was obtained are pakel (9.95%), kopyor (7.40%) and kweni (Mangifera odorata) (2.49%) respectively.

DEVELOPMENT AND VALIDATION OF NOVEL STABILITY INDICATING RP-HPLC METHOD FOR QUANTIFICATION OF TOLVAPTAN IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (03) ◽  
pp. 62-68
Author(s):  
Khaleel Noorbasha ◽  
S. K. Abdul Rahaman
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Reversed Phase ◽  
Hplc Method ◽  
Working Standard ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Bulk Drug

Specific stability-indicating reversed-phase high performance liquid chromatography (HPLC) method has been developed and validated for the quantification of tolvaptan in bulk drug and pharmaceutical dosage form. The optimized conditions for the developed HPLC method are; Inertil ODS-3V column (150 x 4.6 mm, 5.0 mm) maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 40:60%v/v on isocratic mode at flow rate of 1.0 mL/min and detection wavelength 254 nm. The retention time of tolvaptan was found to be 2.59 min with linearity in the concentration range from 37.5 – 225.0 µg/mL, respectively. The mean percentage recovery of tolvaptan was found to be 98.30 – 101.13 %, respectively. The percent relative standard values were less than 2.0 at all the levels and indicates a satisfactory accuracy and precision. The robustness of the method found to meet the acceptance criteria. The stress study against qualified working standard of Tolvaptan, indicated that the developed HPLC method was stability- indicating, conducted as per ICH requirements. The developed method can be handy in the quality control of bulk and pharmaceutical dosage forms.

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