scholarly journals Forced degradation of tacrolimus and the development of a UHPLC method for impurities determination

2019 ◽  
Vol 69 (3) ◽  
pp. 363-380 ◽  
Author(s):  
Tanja Rozman Peterka ◽  
Tina Trdan Lušin ◽  
Jure Bergles ◽  
Zoran Ham ◽  
Rok Grahek ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Thermal Light ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Abstract An ultra-high performance liquid chromatography method for simultaneous determination of tacrolimus impurities in pharmaceutical dosage forms has been developed. Appropriate chromatographic separation was achieved on a BEH C18 column using gradient elution with a total run time of 14 min. The method was applied to analyses of commercial samples and was validated in terms of linearity, precision, accuracy, sensitivity and specificity. It was found to be linear, precise and accurate in the range of 0.05 to 0.6 % of the impurities level in pharmaceutical dosage forms. Stability indicating power of the method was demonstrated by the results of forced degradation studies. The forced degradation study in solution revealed tacrolimus instability under stress alkaline, thermal, light and photolytic conditions and in the presence of a radical initiator or metal ions. The drug was stable at pH 3–5. Solid-state degradation studies conducted on amorphous tacrolimus demonstrated its sensitivity to light, elevated temperature, humidity and oxidation.

DEVELOPMENT AND VALIDATION OF THE REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE ESTIMATION OF GUAIFENESIN IN METHOCARBAMOL API AND ITS PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (5) ◽  
pp. 401
Author(s):  
Mannem Durga Babu ◽  
Kesana Surendrababu
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Solution Stability ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatography Method

Objective: The objective of the study was to develop and validate a novel, specific, precise, and simple reversed-phase high-performance liquid chromatography method for the estimation of guaifenesin present in methocarbamol API and its pharmaceutical dosage forms. Methods: The baseline separation for methocarbamol and guaifenesin was achieved by utilizing a Inertsil ODS C18 (250 mm × 4.6 mm) 5 μm column particle size and an isocratic elution method. The mobile phase contains a mixture of water and acetonitrile in the ratio of 70:30 v/v, respectively. The flow rate of the mobile phase was 1.0 mL/min with a column temperature of 25°C and detection wavelength at 272 nm. The method was validated for a limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and reproducibility with the help of the exhibit and simulated samples. Results: The LOD for guaifenesin was 0.62 μg/mL. The LOQ for guaifenesin was 1.87 μg/mL. The correlation coefficient obtained for impurity was >0.99. The recovery was obtained for impurity was 106.56% at 50%, 95.20% at 100%, and 100.45% at 150%. In tablet analysis, we can found 0.26% (<0.5%). Conclusion: The developed method was validated as per the ICH guidelines with respect to specificity, precision, linearity, accuracy, LOD and quantification, ruggedness, robustness, and solution stability.

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 QUANTIFICATION OF ROPINIROLE HYDROCHLORIDE IN API AND TABLETS BY NOVEL STABILITY-INDICATING RP-HPLC METHOD: IT’S VALIDATION AND FORCED DEGRADATION STUDIES

2019 ◽  
pp. 293-298
Author(s):  
SADASHIVAIAH R. ◽  
Rohith G. ◽  
SATHEESHA BABU B. K.
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Human Error ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Ropinirole Hydrochloride ◽  
Degradation Studies

Objective: A simple, economical, robust and stability-indicating reverse phase high performance liquid chromatography method was developed and validated for the quantification of ropinirole hydrochloride in API and tablets to achieve shorter retention time, to minimize human error by avoiding the use of buffers and weighing procedure and analyze more number of samples in shorter period of time with good accuracy. Methods: The chromatographic conditions for separation of ropinirole hydrochloride was carried out using Gemini NX C18 column (15 cm x 4.6 mm), 5 µm particle size with the mobile phase composing of methanol: acetonitrile (70:30 v/v), delivered at flow rate 0.7 ml/min and UV detection wavelength at 250 nm. Results: The retention time was observed at 2.718 min. The system suitability results were found to be within limits. The method was precise, with lower than 2 %RSD and the calibration curve was linear (r2=1) over a concentration range of 2.5-160 µg/ml. The detection and quantification limit was found to be 0.045 µg/ml and 0.15 µg/ml, respectively. Recovery of the drug was found between 100.09-100.19%. The assay of ropinirole hydrochloride in ROPITOR® and ROPARK® tablets were found to be 100.4 and 103.60 %, respectively. The forced degradation studies were carried out to demonstrate the specificity of the method by exposing the API under conditions of hydrolysis, oxidation, thermal and photolytic as per ICH Q1A(R2) guidelines. Conclusion: The low coefficient of variation and agreeable recovery confirmed that the newly developed method could be employed for routine analysis of ropinirole hydrochloride in API and tablets.

scholarly journals DEVELOPMENT OF ULTRA-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF CAPTOPRIL IN PHARMACEUTICAL DOSAGE FORMS

2017 ◽  
Vol 10 (11) ◽  
pp. 308
Author(s):  
Liliya Logoyda ◽  
Yuliya Kondratova ◽  
Dmytro Korobko ◽  
Yuriy Soroka
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Research Work ◽  
Dosage Forms ◽  
Specific Method ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatography Method

Objective: The objective of this research was to develop more simple, sensitive, accurate, and less expensive analytical methods for the determination of captopril in medicines by Ultra-high-performance liquid chromatography.Materials and Methods: The chromatographic analysis of captopril performed on liquid chromatography Agilent 1290 Infinity II LC System.Results: A simple, rapid, sensitive, and specific method was developed for the determination of captopril by ultra-high-performance liquid chromatography in mono-medicines and pharmaceutical dosage forms in combination with hydrochlorothiazide without previous separation. Satisfactory resolution was achieved using Fused-Core® technology Ascentis Express C18 column (4.6×150 mm) and a mobile phase consisting of methanol and 0.1% solution of trifluoroacetic acid (40/60, v/v) at a flow rate 1.2 mL/minute and the wavelength detection was 220 nm. Ascentis Express columns, based on Fusеd-core pаrticle technоlogy, prоvide more than twice the speed and efficiency of traditiоnal cоlumns at half the backpressure of sub-2-μm columns. The retention time for captopril was 1.345 minute. The validation of this method was based on the ICH and USP guidelines.Conclusion: The results obtained in this research work clearly indicated that the assay was rapid, sensitive and successfully applied to the determination of both drugs in pharmaceutical dosage forms without interference from tablet excipients.

scholarly journals Simultaneous Estimation of Racecadotril and Ofloxacin by Reverse Phase High Performance Liquid Chromatography Method in Pharmaceutical Dosage Forms.

2019 ◽  
Vol 9 (4-s) ◽  
pp. 165-170
Author(s):  
Komal Gupta ◽  
Deepika Sharma ◽  
Pooja Chawla
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatography Method

Background: Racecadotril and Ofloxacin (RACIGYL- O) drug combination are used for the treatment of diarrhea. The drugs have been estimated individually in formulations but no method has been developed for simultaneous estimation of these two drugs as combination. Objective: To develop and validate a high performance liquid chromatography method for the simultaneous estimation of Racecadotril and Ofloxacin in tablet dosage form. Method: A WATERS C18 column (250 x 4.6mm, 5 μm) with mobile phase consisting of acetonitrile, methanol and water 40:40:20v/v (pH adjusted to 2.7 of water with ortho phosphoric acid). The flow rate was 1.0mL/min and effluents were monitored at 210nm. Results: The retention time of RAC and OFL was 4.666 min and 2.551 min respectively. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision, robustness, Limit of Detection (LOD) and Limit of Quantification (LOQ). Conclusion: The method show good reproducibility and recovery with %RSD less than 2. So the proposed method was found to be simple, rapid, precise and accurate and useful for the determination of RAC and OFL in bulk and pharmaceutical dosage forms.   Keywords: RP-HPLC, Racecadotril, Ofloxacin, ICH guidelines.

scholarly journals STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF APIGENIN AND LUTEOLIN FROM ACHILLEA MILLEFOLIUM LINN

2019 ◽  
pp. 169-172
Author(s):  
GOMATHY SUBRAMANIAN ◽  
S.N.MEYYANATHAN ◽  
GOWRAMMA BYRAN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Objective: A stability-indicating reverse-phase high-performance liquid chromatographic method was developed and validated for the analysis of apigenin and luteolin. The degradation behavior of apigenin and luteolin was investigated under different stress conditions as recommended by the International Conference on Harmonization (ICH). Methods: In the present study, a reversed-phase high-performance liquid chromatography method was developed and the resolution of the plant constituents was successfully achieved using Hibar Lichrospher C8 column with ultraviolet detector at a wavelength of 269 nm. The mobile phase consisted of methanol and 0.5% trifluoroacetic acid (80:20 v/v) at a flow rate of 1.0 ml/min. Both apigenin and luteolin were subjected to various stress degradation studies such as oxidation, acid and alkaline hydrolysis, and photolytic degradation. Results: The proposed method was found to be linear (1–5 μg/ml) with the linear correlation coefficient of R2=0.99. Although the degradation products of stressed conditions were not identified, the methods were able to detect the changes due to stress condition. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. Forced degradation studies on apigenin and luteolin give information about their storage and intrinsic stability conditions considering the advanced pharmaceutical aspects of formulations.

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