Development and Validation of a Stability-Indicating Chromatographic Method for the Determination of Indacaterol Maleate with Glycopyrronium Bromide in Mixture

2019 ◽  
Vol 15 (7) ◽  
pp. 694-702
Author(s):  
Sonia Talaat Hassib ◽  
Hanaa Abdelmenem Hashem ◽  
Marwa Ahmed Fouad ◽  
Nehal Essam Eldin Mohamed
Keyword(s):  
Chromatographic Method ◽  
Degradation Products ◽  
Reversed Phase ◽  
Chronic Obstructive ◽  
Forced Degradation ◽  
Uv Detector ◽  
Obstructive Pulmonary Disease ◽  
Mortality And Morbidity ◽  
Glycopyrronium Bromide

Introduction: (COPD) Chronic Obstructive Pulmonary Disease is a partially reversible and treatable lung disease, characterized by progressive limitation of airflow. It is one of the main causes of mortality and morbidity worldwide. Methods: An easy, precise and selective reversed-phase liquid chromatographic method, with stabilityindicating assay was established and validated for the determination of indacaterol maleate and glycopyrronium bromide in the mixture. In addition, a forced degradation study was performed for indacaterol maleate, comprised of hydrolysis by acid and base, degradation by oxidation and heat, and photo-degradation. Separation and forced degradation were done by isocratic elution using a reversed phase phenyl column and (methanol: phosphate buffer) at ratio (65:35, v/v) with 3.5 pH buffer as an eluent at 1 mL min-1 as a flow rate. Quantitation was accomplished using a UV detector at 210 nm. Results: The method showed good separation of glycopyrronium bromide, indacaterol maleate and its degradation products. Accuracy, linearity, and precision were acceptable over 10-160 µg mL-1 and 10- 80 µg mL-1 concentration range for indacaterol maleate and glycopyrronium bromide, respectively. Conclusion: The proposed method does not require any previously done separation steps, making it applicable for the analysis of the drugs under investigation in their pharmaceutically marketed preparations.

Stability-indicating LC method for the determination of cephalothin in lyophilized powder for injection

2014 ◽  
Vol 6 (12) ◽  
pp. 4437-4445 ◽  
Author(s):  
Karen de Souza Rugani ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Liquid Chromatography ◽  
Degradation Products ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Antimicrobial Compound ◽  
Reversed Phase Liquid Chromatography ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Phase Liquid

A stability-indicating gradient reversed phase liquid chromatography (RP-LC) method has been developed for the quantitative determination of cephalothin (CET), an antimicrobial compound, in the presence of its impurities and degradation products generated from forced degradation studies.

scholarly journals A Stability Indicating UPLC Method for the Determination of Tramadol Hydrochloride: Application to Pharmaceutical Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura B. Vinay ◽  
Hosakere D. Revanasiddappa ◽  
Cijo M. Xavier ◽  
Pavagada J. Ramesh ◽  
Madihalli S. Raghu
Keyword(s):  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Tramadol Hydrochloride ◽  
Stability Indicating

The use of Ultra Performance Liquid Chromatography (UPLC), with a rapid 5-minute reversed phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for tramadol hydrochloride (TMH) is demonstrated. A simple, precise and accurate stability-indicating isocratic UPLC method was developed for the determination of TMH in bulk drug and in its tablets. The method was developed using Waters Aquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogen phosphate buffer of pH 2.8 and an equal volume of acetonitrile (60 : 40 v/v). The eluted compound was detected at 226 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–300 μg mL−1 TMH with regression coefficient (r) value of 0.9999. The limit of detection (S/N =3) was 0.08 μg mL−1 and the limit of quantification (S/N =10) was 0.2 μg mL−1. Forced degradation of the bulk sample was conducted an accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. TMH was found to degrade significantly in acidic, basic and oxidative stress conditions and stable in thermal, hydrolytic and photolytic conditions.

Identification and characterization of degradation products of indacaterol using liquid chromatography/mass spectrometry

2020 ◽  
Vol 26 (6) ◽  
pp. 425-431
Author(s):  
Naga Veera Yerra ◽  
S Babu Dadinaboyina ◽  
LSSN Vigjna Abbaraju ◽  
MVN Kumar Talluri ◽  
Jagadeshwar Reddy Thota
Keyword(s):  
Degradation Products ◽  
Thermal Conditions ◽  
Active Pharmaceutical Ingredient ◽  
Stress Conditions ◽  
Chronic Obstructive ◽  
Forced Degradation ◽  
Obstructive Pulmonary Disease ◽  
Guide Lines ◽  
Identification And Characterization

Indacaterol (IND), 5-[2-[(5,6-Diethyl-2,3-dihydro-1H-inden-2-yl)amino]-1-hydroxyethyl]-8-hydroxyquinolin-2(1H)-one, is an active pharmaceutical ingredient (API) which is used to treat chronic obstructive pulmonary disease (COPD). We followed the International Council for Harmonization (ICH) guide lines to study the degradation behavior of IND under various stress conditions. Stressed degradation of the drug was performed under hydrolytic (alkaline, acidic and neutral), photolytic, oxidative and thermal conditions. Identification and characterization of IND and its forced degradation products (DPs) were demonstrated by using LC-HRMS and MS/MS method. A total of three DPs (DP1-DP3) were identified and characterized. The IND was found to be stable under photolytic, oxidative and thermal conditions, whereas it produced three DPs in acidic, basic and neutral hydrolytic stress conditions.

A VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF AZELNIDIPINE AND ITS IMPURITIES IN PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (08) ◽  
pp. 70-76
Author(s):  
Pavani Peddi ◽  
S. L. Tulasi ◽  
N. Usha Rani ◽  
T. Raja Rajeswari
Keyword(s):  
Degradation Products ◽  
Impurity Content ◽  
Hplc Method ◽  
Stability Study ◽  
Forced Degradation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Formulation Analysis

A novel simple, rapid, sensitive and stability-indicating RP-HPLC method was developed and validated for the determination of azelnidipine (ALDP) and its impurities 1 and 2. Resolution of drug, its potential impurities and degradation products were achieved by RP-HPLC on was performed on Prontosil ODS C18 column (250 mm x 4.6 mm, 5µ) using a mobile phase consisting of methanol and 0.1M sodium acetate 40: 60 (v/v) at a flow rate of 1 ml/min and 231 nm of UV detector. Validation of the method was performed along with formulation analysis and forced degradation studies. The calibration curves of ALDP were linear over a concentration range of 50-300 µg/mL. The method was rapid with a retention time of the impurity 2, impurity and ALDP observed at 3.60, 5.15 and 6.90 min, respectively. The method was applied for the impurities determination in drug tablets and for degradation products determination in a stability study of ALDP. The impurity content in the tablets was quantified as 0.1% of total drug. The method can also be used for rapid and accurate quantification of ALDP in its tablets during stability testing.

scholarly journals Determination of Mesalamine Related Impurities from Drug Product by Reversed Phase Validated UPLC Method

2011 ◽  
Vol 8 (1) ◽  
pp. 131-148 ◽  
Author(s):  
Trivedi Rakshit Kanubhai ◽  
Patel Mukesh C ◽  
Kharkar Amit R
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Release Formulation ◽  
Delayed Release ◽  
Related Substances

In the present study gradient reversed-phase UPLC method was developed for simultaneous determination and separation of impurities and degradation products from drug product. The chromatographic separation was performed on acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 µm) using gradient elution. Other UPLC parameters which were optimised are flow rate, 0.7 mL/min; detection wavelength, 220 nm; column oven temperature, 40°C and injection volume 7 µL. Stability indicating capability was established by forced degradation experiments and separation of known degradation products. The method was validated as per International Conference on Harmonization (ICH) guideline. For all impurities and mesalamine, LOQ (limit of quantification) value was found precise with RSD (related standard daviation) of less than 2.0%. In essence, the present study provides an improved low detection limit and lower run time for evaluation of pharmaceutical quality of mesalamine delayed-release formulation. Moreover, the developed method was successfully applied for quantification of impurities and degradation products in mesalamine delayed-release formulation. The same method can also be used for determination of related substances from mesalamine drug substance.

Simultaneous Liquid Chromatographic Determination of Fenamiphos and Its Metabolites in Soil

1992 ◽  
Vol 75 (1) ◽  
pp. 62-65 ◽  
Author(s):  
R Khazanchi ◽  
S Walia ◽  
S K Handa
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method has been developed for the determination of fenamiphos and the metabolites fenamiphos sulfoxide, fenamiphos sulfone, 3-methyl-4-(methylthlo)- phenol, and 3-methyl-4-(methylsulflnyl)phenol. Trace quantities of the nematlclde and Its metabolites In soil can be determined simultaneously. The limit of detection of the method was 5 ppm. Recoveries of fenamiphos and Its degradation products at fortification levels of 25,50, and 100 ppm ranged from 99.2 to 100.8%. Standard deviations ranged from 0.29 to 0.70 ppm.

scholarly journals Determination of Cefdinir by a Stability-Indicating Liquid Chromatographic Method

2005 ◽  
Vol 88 (6) ◽  
pp. 1661-1665 ◽  
Author(s):  
Tushar N Mehta ◽  
Gunta Subbaiah ◽  
Kilambi Pundarikakshudu
Keyword(s):  
Chromatographic Method ◽  
Degradation Products ◽  
Reversed Phase ◽  
Stability Indicating ◽  
Pharmaceutical Ingredients ◽  
Degraded Samples ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A simple, fast, specific, stability-indicating, and precise reversed-phase liquid chromatographic method was developed for the determination of Cefdinir in its different dosage forms, i.e., capsules and suspensions. The method was developed and optimized by analyzing the placebo preparation, formulations, and degraded samples of the drug substance according to the International Conference on Harmonization. The proposed method can successfully separate the drug from degradation products formed under stress conditions along with pharmaceutical ingredients such as preservatives. The developed method was used successfully to determine Cefdinir in capsules and Insta-use suspensions. The developed method was found to be linear for a concentration range of 6–14 μg/mL. Average recoveries obtained with the method were 99.3 ± 0.4 and 99.6 ± 0.4% for Insta-use suspensions and capsules, respectively. The method was shown to be specific, precise, and robust.

scholarly journals Development and Validation of Stability-Indicating RP-UPLC Method for the Determination of Methdilazine in Bulk Drug and in Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Madihalli S. Raghu ◽  
Kanakapura Basavaiah ◽  
Cijo M. Xavier ◽  
Kudige N. Prashanth
Keyword(s):  
Limit Of Detection ◽  
Bulk Sample ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Bulk Drug

A simple, precise, and accurate, and stability-indicating isocratic Ultraperformance Liquid Chromatography (UPLC) method was developed for the determination of methdilazine hydrochloride (MDH) in bulk drug and in its tablets. The use of UPLC, with a rapid 5-minute-reversed-phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for MDH, is demonstrated. The method was developed using Waters Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogenorthophosphate and 1-pentane sulphonic acid buffer of pH 4.0 and acetonitrile (60 : 40 v/v). The eluted compound was detected at 254 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–80 μg mL−1 MDH with regression coefficient () value of 0.9999. The limit of detection () was 0.2 μg mL−1 and the limit of quantification () was 0.5 μg mL−1. Forced degradation of the bulk sample was conducted in accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal, and photolytic degradations were used to assess the stability indicating power of the method. The drug was found to be stable in acidic, basic, thermal, hydrolytic, and photolytic stress conditions and showed slight degradation in oxidative stress condition.

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