A pH-Stability Study of Phoslactomycin B and Analysis of the Acid and Base Degradation Products

A trouble-free, simple, specific and highly sensitive stability indicating phase HPLC method was developed for concurrent assessment of Daclatasvir and Sofosbuvir in pure and in their combined tablet formulation. An effectual separation was accomplished by using XDB Phenyl (250 x 4.6mm, 5µ,100 A0) column, mobile phase composition of Acetonitrile: buffer(0.1%v/v Trifluoroaceticacid in water) (50:50 v/v) and isocratic elution at a flow rate of 1ml/min and detection wavelength of 275nm. The extreme stress conditions like hydrolysis with acid and base, peroxide oxidation, thermal decomposition were used as per ICH specifications to assess the stability of the analytes in bulk and dosage forms. The retention times of Daclatasvir and Sofosbuvir were found at 2.8 and 3.7min respectively. The proposed method has linear response in the concentration ranges from 12 to 36µg/ml and 80 to 240 µg/ml for Daclatasvir and Sofosbuvir respectively. The detection and quantification limits calculated as 2.5μg/ml and 7.8μg/ml for DCL, 5.2μg/ml and 15.8μg/ml SOF respectively. All the method validation parameters were met the acceptance limits of Q2 specifications of ICH procedures. The degradation products produced by forced degradation studies were have good resolution from Daclatasir and Sofosbuvir peaks, which represents the methods stability. The proposed RP-HPLC method was highly sensitive, precise, stability indicating and economical. That’s why the method has the capacity to employ in the pharmaceutical manufacturing of Daclatasvir and Sofosbuvir and routine analysis in quality control department.

Download Full-text

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

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2017v9i1.16076 ◽

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.

Download Full-text

Stability-Indicating Validated HPLC Method for Simultaneous Determination of Oral Antidiabetic Drugs from Thiazolidinedione and Sulfonylurea Groups in Combined Dosage Forms

Journal of AOAC International ◽

10.1093/jaoac/93.4.1086 ◽

2010 ◽

Vol 93 (4) ◽

pp. 1086-1092 ◽

Cited By ~ 1

Author(s):

Anna Gumieniczek ◽

Anna Berecka ◽

ukasz Komsta

Keyword(s):

Simultaneous Determination ◽

Mobile Phase ◽

Uv Light ◽

Degradation Products ◽

Dosage Forms ◽

Hplc Method ◽

Base Temperature ◽

Stability Indicating ◽

Acid And Base

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.

Download Full-text

Development and Validation of Stability Indicating High-Performance Thin-Layer Chromatographic (HPTLC) Method for Quantification of Asiaticoside from Centella asiatica L. and its Marketed Formulation

Journal of AOAC International ◽

10.5740/jaoacint.18-0381 ◽

2019 ◽

Vol 102 (4) ◽

pp. 1014-1020

Author(s):

Lisa J Patel ◽

Manan A Raval ◽

Samir G Patel ◽

Archita J Patel

Keyword(s):

High Performance ◽

Degradation Products ◽

Degradation Kinetics ◽

Centella Asiatica ◽

Stability Study ◽

Cns Disorders ◽

Marker Compound ◽

Plant Powders ◽

Development And Validation ◽

Hptlc Method

Abstract Background: Ayurvedic medicines help in healing disease with fewer undesirable effects in comparison with an allopathic system of medicine to treat central nervous system (CNS) disorders, as the latter is more expensive. Centella asiatica L. is often used in Ayurvedic formulations for the treatment of CNS disorders. Objective: A stability test using an HPTLC method for the estimation of an important marker asiaticoside (ASI) from C. asiatica powder and marketed formulation was developed. Methods: The marker compound ASI from plant powders and marketed formulations were resolved using toluene–ethyl acetate–methanol–glacial acetic acid (2+7+3+1, v/v/v/v) as the mobile phase and then was derivatized. The plant powder and marketed formulation were also subjected to stability studies. Results: The Rf value of ASI was found in range of 0.43–0.47 for the standard ASI, plant powder, and marketed formulation. It was found that the plant powder and formulation exhibited first-order degradation kinetics. Conclusions: The contents of ASI in the formulation (Churna) and its flow characters reduced at the end of the 6 months during an accelerated stability study. The developed method can be used to quantify ASI in the presence of its degradation products. Highlights: The developed method helps in determining batch to batch variation in the content of ASI in herbal formulations.

Download Full-text

Stability-indicating UPLC-PDA Method for Ambrisentan Tablets and Identification of a Main Degradation Product by UPLC-MS/MS

Current Pharmaceutical Analysis ◽

10.2174/1573412914666181003140449 ◽

2019 ◽

Vol 16 (1) ◽

pp. 55-63

Author(s):

Rodolfo Ortigara ◽

Martin Steppe ◽

Cássia Virginia Garcia

Keyword(s):

Degradation Product ◽

Degradation Products ◽

Stability Study ◽

Drug Degradation ◽

Mode Waters ◽

System Suitability ◽

Main Degradation Product ◽

Pulmonary Arterial ◽

Gradient Mode ◽

Drug Quality Control

Background: Ambrisentan is a drug used to treat the pulmonary arterial hypertension symptoms, commercialized as coated tablets. Drug quality control is an essential part for the development and release of drugs for consumption; however, there are few studies related to the proposition of analytical methods and stability study for ambrisentan. Objective: The development of an UPLC assay of ambrisentan in tablets with degradation product`s elucidation was proposed. Methods: Tests with different solvents and chromatographic columns were carried out, achieving an optimal condition using mobile phase in gradient mode, Waters® BEH C18 column and detection at 260 nm. Results: Satisfactory system suitability was obtained (theoretical plates, sensitivity and resolution among peaks), with a reduced analysis time (6 minutes). The method was validated in accordance with the international guidelines and it demonstrated adequate specificity, either for the drug assay as for the identification and quantification of degradation product. It showed linearity (r= 0.999), accuracy (degradation products recovery: 98.47 - 102.44; assay recovery: 99.98 - 104.32%) and precision (RSD: 0.69), with limits of quantification and detection in suitable magnitude in order to evaluate possible drug degradation. Conclusion: UPLC method demonstrated to be fast with satisfactory robustness. The main ambrisentan degradation product formed under thermal stress conditions was elucidated by UPLC-MS/MS and its structure was suggested.

Download Full-text

Determination of Rosuvastatin in the Presence of Its Degradation Products by a Stability-Indicating LC Method

Journal of AOAC International ◽

10.1093/jaoac/88.4.1142 ◽

2005 ◽

Vol 88 (4) ◽

pp. 1142-1147 ◽

Cited By ~ 14

Author(s):

Tushar N Mehta ◽

Atul K Patel ◽

Gopal M Kulkarni ◽

Gunta Suubbaiah

Keyword(s):

Degradation Products ◽

Stability Study ◽

Tablet Formulation ◽

Assay Method ◽

Forced Degradation ◽

Degradation Study ◽

Stability Indicating ◽

Degraded Samples ◽

Accelerated Stability

Abstract A forced degradation study was successfully applied for the development of a stability-indicating assay method for determination of rosuvastatin Ca in the presence of its degradation products. The method was developed and optimized by analyzing the forcefully degraded samples. Degradation of the drug was done at various pH values. Moreover, the drug was degraded under oxidative, photolytic, and thermal stress conditions. Mass balance between assay values of degraded samples and generated impurities was found to be satisfactory. The proposed method was able to resolve all of the possible degradation products formed during the stress study. The developed method was successfully applied for an accelerated stability study of the tablet formulation. The major impurities generated during the accelerated stability study of the tablet formulation were matches with those of the forced degradation study. The developed method was validated for determination of rosuvastatin Ca, and the method was found to be equally applicable to study the impurities formed during routine and forced degradation of rosuvastatin Ca.

Download Full-text

HPLC Method for Monitoring of Degradation Products in Picoplatin Stability Study

Chromatographia ◽

10.1007/s10337-011-1938-1 ◽

2011 ◽

Vol 73 (S1) ◽

pp. 131-135

Author(s):

Jitka Housková ◽

Michaela Hrdá ◽

Kamila Syslová ◽

Petr Novotný ◽

Petr Kačer

Keyword(s):

Degradation Products ◽

Hplc Method ◽

Stability Study

Download Full-text

Ultra performance liquid chromatographic method for simultaneous quantitation of degradation products of telmisartan and hydrochlorothiazide in combination dosage form

International Journal of Research in Pharmaceutical Sciences ◽

10.26452/ijrps.v11i2.2148 ◽

2020 ◽

Vol 11 (2) ◽

pp. 2070-2082

Author(s):

Narasimha Reddy G P ◽

Sreenivasulu Reddy T ◽

Sidda Reddy K ◽

Shashi Kumar K N

Keyword(s):

Mobile Phase ◽

Method Development ◽

Limit Of Detection ◽

Degradation Products ◽

Drug Product ◽

Wave Length ◽

Stability Study ◽

Limit Of Quantification ◽

Pharmaceutical Dosage Forms ◽

Stability Indicating

This work is intended to thrive a stability indicating Ultra performance liquid method for the estimation of (TLM) and (HCTZ) and degradation products pharmaceutical dosage forms. Separation was carried out on Zorbax Eclipse XDB C-18(50 x 2.1 mm, 1.7 ) column using a gradient method. Mobile phase A is 10mM KH2PO4 having 1% (v/v) of and mobile phase B is used in this work. 0.5 / minute is the flow of rate and at 271nm noticed wave length is monitored. Method development trails were carried out on six different columns. For specificity, limit of quantification, limit of detection, linearity, accuracy, method precision, robustness and stability this method is validated. Correlation coefficient of the impurities is more than 0.99. Stability indicating method confirmed that there were no interference of all impurities of TLM and HCTZ. Hence, developed LC method was stability indicating and well applied for drug product stability study as well as to quality monitoring.

Download Full-text

Degradation study of stevioside using RP-HPLC and ESI-MS/MS

Malaysian Journal of Fundamental and Applied Sciences ◽

10.11113/mjfas.v14n1-2.956 ◽

2018 ◽

Vol 14 (1-2) ◽

pp. 138-141 ◽

Cited By ~ 2

Author(s):

Yohanes Martono ◽

Abdul Rohman ◽

Sudibyo Martono ◽

Sugeng Riyanto

Keyword(s):

Degradation Products ◽

Stress Factors ◽

Base Hydrolysis ◽

Esi Ms ◽

Rp Hplc ◽

Base Solution ◽

Acid And Base ◽

Dry Heating ◽

H2o2 Oxidation ◽

The Stability

Stevioside is very potential to be an antidiabetic pro-drug. In processing, the active ingredient may be degraded. This research conducted a study of the degradation of stevioside on several stress factors such as acid and base hydrolysis; exposure to UV rays, thermal heating and oxidation using RP-HPLC. The degradation products were identified using ESI-MS/MS. Hydrolysis of acid-base solution and exposure to UV254 nm rays caused the breakdown of glycoside bonds in the analyte. Stevioside was unstable in dry heating at 105oC for 48 hours due to degradation of 91%. Stevioside was oxidized under H2O2 oxidation for 48 hours. Based on the ESI-MS/MS analysis, the identified stevioside degradation products were [M-H] ̶ with m/z = 803 as stevioside; [M-H] ̶ with the value of m/z = 641 as steviolbioside; [M-H] ̶ with m/z = 479 as steviolmonoside; [M-H] ̶ with m/z = 317 as steviol. Termination of glucose was characterized by fragmentation [M-162] ̶.Our study provides a basic view on the stability and degradation characteristics of stevioside, and demonstrates the formation of degradation products.

Download Full-text

pH Stability Study of Lectin from Black Turtle Bean (Phaseolus vulgaris) as Influenced by Guanidinium–HCl and Thermal Treatment

Protein and Peptide Letters ◽

10.2174/0929866521666140909155556 ◽

2014 ◽

Vol 22 (1) ◽

pp. 45-51 ◽

Cited By ~ 7

Author(s):

Shudong He ◽

Benjamin Simpson ◽

Michael Ngadi ◽

Sophia Xue ◽

John Shi ◽

...

Keyword(s):

Phaseolus Vulgaris ◽

Thermal Treatment ◽

Stability Study ◽

Ph Stability

Download Full-text