scholarly journals Monitoring of thermal and oxidation stability of sodium picosulfate by modified RP-HPLC method

2010 ◽  
Vol 16 (1) ◽  
pp. 103-110 ◽  
Author(s):  
Ivana Savic ◽  
Goran Nikolic ◽  
Valentina Marinkovic ◽  
Ivan Savic
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Oxidation Stability ◽  
Bulk Sample ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Sodium Picosulfate ◽  
Bulk Drug

A selective, precise and stability-indicating, modified high performance liquid chromatographic method for the analysis of sodium picosulfate both as a bulk drug and in formulations was developed and validated. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one. The chromatographic separation was achieved on a ZORBAX Eclipse XDB C-18 analytical column. The mobile phase consisted of phosphate buffer (pH 7):acetonitrile (85:15 v/v). The absorbance was monitored with a DAD detector at 263 nm. The flow rate was 1.5 mL min-1. Statistical analysis proved the method is repeatable, selective, and accurate for estimation of sodium picosulfate in the presence its degradation product. Forced degradation studies were performed on bulk sample of sodium picosulfate using heat (25, 40, 60 and 80 ?C) and oxidation (0.1, 0.5 and 1% v/v hydrogen peroxide). The proposed method was successfully applied, with excellent recovery, to the analysis of a pharmaceutical formulation (Sodium picosulfate, Zdravlje-Actavis, Serbia).

scholarly journals SIMULTANEOUS QUANTIFICATION OF PENTAZOCINE AND NALOXONE BY STABILITY INDICATING REVERSE-PHASE-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD

2019 ◽  
pp. 257-262
Author(s):  
RAMA KUMAR KANDULA ◽  
RAJA SUNDARARAJAN
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Alkali Hydrolysis ◽  
Liquid Chromatographic

Objective: The objective of the study was to develope a stability indicating high-performance liquid chromatographic (HPLC) method for simultaneous assay of pentazocine and naloxone in bulk and tablets. Methods: Pentazocine and naloxone were analyzed on Dionex C18 column using 0.1M K2HPO4 buffer (pH 4.0) and methanol (60:40, v/v) as the mobile phase. The concentration of pentazocine and naloxone was quantified by photodiode array detector set at 248 nm. The method was validated in compliance with ICH rules. Pentazocine and naloxone tablet formulation was subjected to forced degradation such as acid, neutral and alkali hydrolysis, oxidation, photo, and thermal degradation. Results: The method was linear, with R2=0.9999 in the concentration range 100–300 μg/ml for pentazocine and R2=0.9995 in the concentration range 1–3 μg/ml for naloxone. The level of detection and quantification was 0.097 μg/ml and 0.322 μg/ml for pentazocine and 0.0073 μg/ml and 0.0243 μg/ml for naloxone, respectively. The degraded products are resolved well from pentazocine and naloxone with significantly different retention time values. From validation results, it was proved that the method is selective, precise, robust, and accurate for the estimation of pentazocine and naloxone simultaneously. Conclusion: The developed stability-indicating HPLC method can be applied for quantitative determination of pentazocine and naloxone in tablets.

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.

Development and Validation of a Stability-Indicating HPLC Method for the Analysis of Cabazitaxel in Jevtana® Concentrate-Solvent Leftover Samples

2020 ◽  
Vol 16 ◽  
Author(s):  
Hedvig Arnamo ◽  
Michel Hillebrand ◽  
Alwin Huitema ◽  
Bastiaan Nuijen ◽  
Hilde Rosing ◽  
...  
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Uv Light ◽  
Degradation Products ◽  
Physical Stability ◽  
Solvent Mixture ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method

Aim/Background: In this study, a stability-indicating method of the anticancer agent cabazitaxel was developed and validated. This method will be used to determine the chemical stability of commercially available concentrate-solvent mixture cabazitaxel (Jevtana®) to examine the possibility of multi-dosing from the same product vial after storage. The impossibility to re-use leftovers today is contributing to an unnecessary and significant financial waste. Methods: A forced degradation study of cabazitaxel was performed under different conditions to produce degradation products. Acidic, basic, oxidation, heat, and ultraviolet (UV) light conditions were tested. The method to determine the stability was developed so that potential degradation products would be shown in the UV spectra after separation from cabazitaxel with a C18 column in a high-performance liquid chromatography (HPLC) system. The only degradation product occurring during storage in room temperature and ambient light was identified by accurate mass Orbitrap Mass Spectrometry. Results/Conclusion: A stability-indicating method for cabazitaxel (Jevtana ®) concentrate-solvent mixture has been developed. We demonstrated that this method can be applied to stability studies with the purpose of multi-dosing cabazitaxel from a chemical/physical stability perspective within the tested period of time and conditions. As an addition, the only naturally occurring degradation product found has been identified and a degradation reaction has been suggested.

scholarly journals A validated stability indicating RP-HPLC method for the quantification of Canagliflozin

2018 ◽  
Vol 9 (1) ◽  
pp. 206
Author(s):  
Sreenivasulu S ◽  
Rameswara Rao M ◽  
Chandra Sekhar KB
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Plate Count ◽  
Forced Degradation ◽  
Chromatographic Study ◽  
Limit Of Quantification ◽  
Stability Indicating

A simple, authentic and stability indicating high performance liquid chromatographic method for determination of Canagliflozin in bulk and pharmaceutical formulations was developed and validated as per ICH Q2 R1 Guidelines, A C18 Column (250mm length×4.6 mm diameter x 5 μm particle size) with a mobile phase consisting of Acetonitrile: 1-octanesulphonic acid in a ratio of 70:30 v/v was employed for the chromatographic study. A flow rate of 1.0 mL/min with an injection volume of 20 μL was selected for this study and the proposed method was validated with different parameters such as Linearity, Precision, Accuracy, Robustness, Ruggedness, Limit of Detection (LOD) and Limit of Quantification (LOQ). Canagliflozin was eluted at 3.4 ± 0.5 min and detected at 245 nm. The method is linear over the concentration range of 10-100 μg/mL with correlation co-efficient r = 0.9997. The plate count and tailing factor was found 5398 and 1.05 respectively. The LOD and LOQ were found to be 0.0170 μg/mL and 0.1705 μg/mL respectively. The percentage recovery was achieved in the range of 98-102%, which was within the acceptance criteria. Developed method was employed to determine the amount of Canagliflozinpresent in dosage form (Sulisent). The stabilityof the method was demonstrated by forced degradation studies of drug in which it was degraded under conditions of hydrolysis (acidic and alkaline), oxidation, photolytic and thermal stress as per ICH guideline Q1A (R2).

scholarly journals A validated stability indicating HPLC method for the determination of process-related impurities in pantoprazole bulk drug and formulations

2013 ◽  
Vol 49 (1) ◽  
pp. 175-184 ◽  
Author(s):  
Saurabh Pandey ◽  
Preeti Pandey ◽  
Durgesh Mishra ◽  
Umesh Kumar Singh
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Assay Method ◽  
Stability Indicating ◽  
Related Impurities ◽  
Short Run ◽  
Bulk Drug ◽  
Liquid Chromatographic

A stability-indicating high-performance liquid chromatographic (HPLC) method was developed with short run time and validated for the assay of process related impurities of pantoprazole in bulk form. Resolution of drug, its potential impurities and degradation products were achieved on a Hypersil ODS column utilizing a gradient with 0.01 M phosphate buffer of pH 7 and acetonitrile as eluent, at the detection wavelength of 290 nm. Flow rate was set at 1 mL min-1. The procedure was found to be specific, linear (r=0.999), recovery (97.9-103%), LOD (0.043-0.047 µgmL-1), LOQ (0.13-0.14 µgmL-1) and robust. Acceptable robustness indicates that the assay method remains unaffected by small but deliberate variations. Pantoprazole was found to degrade in acidic, oxidative and under photolytic stress conditions. The drug was stable to alkaline and dry heat conditions. This method has been successively applied to pharmaceutical formulation and no interference from the excipients was found.

QBD ASSISTED RP-HPLC METHOD FOR IDENTIFICATION OF TERAZOSIN IN BULK DRUG AND PHARMACEUTICAL SAMPLE

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (03) ◽  
pp. 19-26
Author(s):  
C. Dhal ◽  
◽  
D. Rajput ◽  
V. Tiwari ◽  
A. Teotia ◽  
...  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Drugs ◽  
Reliable Technique ◽  
Rp Hplc ◽  
Bulk Drug ◽  
Liquid Chromatographic

Reversed Phase High Performance Liquid Chromatographic (RP-HPLC) proves to be a convenient and reliable technique for the identification of various compounds, such as pharmaceutical drugs of chemical as well as phyto origin, food compounds and others. Analytical method for the estimation of alpha-1 antagonist terazosin, a potent anti-hypertensive agent for enlarged prostate, was developed, optimized for the best fit condition using statistical software Minitab and validated as per International Conference on Harmonization (ICH) Q2 (R1) guidelines. Partitioning of the desired molecule was achieved on Agilent Zorbax C18 column with dimensions of 250 mm X 4.6 mm and a particle size 5μm against mobile phase containing acetate buffer adjusted to pH 6.0 and acetonitrile (ACN) in a ratio 30:70 (V/V), run isocratically for sufficient time. The linear model was established between 50 – 250 ppm with a regression coefficient (r2) of 0.9971 and with detection (LOD) and quantification limit (LOQ) of 17.754 ppm and 53.802 ppm, respectively. The method was precise, accurate, robust and able to distinguish between the adduct generated during forced degradation studies.

scholarly journals Monitoring of the photochemical stability of carvedilol and its degradation products by the RP-HPLC method

2007 ◽  
Vol 72 (1) ◽  
pp. 37-44 ◽  
Author(s):  
Jelena Stojanovic ◽  
Sote Vladimirov ◽  
Valentina Marinkovic ◽  
Dragan Velickovic ◽  
Predrag Sibinovic
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Uv Detector ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Liquid Chromatographic

A sensitive, selective, precise and stability-indicating, new high-performance liquid chromatographic method for the analysis of carvedilol both as a bulk drug and in formulations was developed and validated. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. The method was validated for linearity, selectivity, precision, robustness, LOD, LOQ and accuracy. The chromatographic separation was achieved on a Chromolit RP8e, 100x4.6 mm, analytical column. The mobile phase consisted of a mixture of acetonitrile and water (45:55, V/V) (pH 2.5), pH adjusted with formic acid. The absorbance was monitored with a UV detector at 280 nm and the temperature of the analyses was 40?C. The flow rate was 0.5 mL/min. The linearity (r? 0.999), reproducibility (0.68-1.27 %) and recovery (99.71-101.58) were found to be satisfactory. This method enables the simultaneous determination of carvedilol and its degradation products, as well as stability. .

FORCED DEGRADATION STUDIES OF OLMESARTAN MEDOXOMIL AND CHLORTHALIDONE: DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING RP‑HPLC METHOD

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (03) ◽  
pp. 39-45
Author(s):  
A Sherje ◽  
A. Sonalkar ◽  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Olmesartan Medoxomil ◽  
The United States ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Uv Detector ◽  
Tablet Dosage

A reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of olmesartan medoxomil (OLME) and chlorthalidone (CHLOR) in tablet dosage form. The analysis was performed on Inertsil ODS C18 (250 x 4.6 mm, 5 μ) using KH2PO4 phosphate buffer (pH) and acetonitrile as mobile phase in the proportion of 60: 40 v/v at flow rate of 1.0 mL/min. Detection of drugs was carried out in isocratic mode using UV detector at 275 nm. The retention time of OLME and CHLOR was 13.9 ± 0.1 min. and 4.4 ± 0.5 min., respectively and the total run time was 20 min. The method was validated according to the requirements of the United States Pharmacopeia. The percentage recoveries was found to be in the range of 98.9 - 100.7%. The method was successfully applied to the assay of OLME and CHLOR in tablet dosage form.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

scholarly journals ESTIMATION OF AMLODIPINE BESYLATE AND IRBESARTAN IN PHARMACEUTICAL FORMULATION BY RP-HPLC WITH FORCED DEGRADATION STUDIES

2019 ◽  
pp. 159-167 ◽  
Author(s):  
T Hemant Kumar ◽  
CH. ASHA ◽  
D. GOWRI SANKAR
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Amlodipine Besylate ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Liquid Chromatographic

Objective: To develop and validate a simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method with forced degradation studies for the simultaneous estimation of amlodipine besylate and irbesartan in the pharmaceutical formulation. Methods: The chromatographic separation of the two drugs were achieved using Enable C 18G column (250 ×4.6 mm; 5 µm) in isocratic mode with mobile phase consisting of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, % v/v) with a flow rate of 0.6 ml/min. Ultraviolet(UV) detection was carried out at 238 nm. The proposed method was validated for linearity, range, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The tablet formulation was subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis. Results: The retention time for amlodipine besylate and irbesartan were found to be 5.512 and 6.321 min respectively. Linearity was observed over a concentration range 4-32 µg/ml for amlodipine besylate (r2 =0.9999) and 10-70 µg/ml for Irbesartan (r2 =0.9998). The % relative standard deviation (RSD) for Intraday and Interday precision was found to be 0.436 and 0.699 for amlodipine besylate and 0.435 and 0.30 for irbesartan. Amlodipine besylate shown stability towards acidic and thermal whereas in basic, oxidative and photolytic it shown less stability in which it degraded to more extent. Irbesartan shown stability towards thermal conditions whereas in remaining conditions it degrades to more extent especially in oxidative conditions. Conclusion: The developed reverse phase high performance liquid chromatographic (RP-HPLC) method was also found to be simple, precise and sensitive for the simultaneous determination of amlodipine besylate and irbesartan in the tablet dosage form.

Sign in / Sign up

Export Citation Format

Share Document