Development of a Stability-Indicating RP-HPLC Method for Determination of Rupatadine and its Degradation Products in Solid Oral Dosage Form

Abstract An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 4.6 mm id) maintained at 30C. The mobile phase consisted of acetonitrilewater (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5200 g/mL (r2 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19, with bias lower than 1.81. The LOD and LOQ were 0.39 and 0.5 g/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.

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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.

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Development of Stability Indicating RP-HPLC Method for Determination of Levosulpiride Hydrochloride In Bulk And Pharmaceutical Dosage Form

International Journal of Advances in Pharmaceutical Analysis ◽

10.7439/ijapa.v2i2.18 ◽

2012 ◽

Vol 2 (2) ◽

Author(s):

Usmangani K. Chhalotiya

Keyword(s):

Dosage Form ◽

Hplc Method ◽

Pharmaceutical Dosage Form ◽

Stability Indicating ◽

Rp Hplc

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Development and Validation of Two Robust Stability-Indicating Chromatographic Methods for Determination of Metolazone in Drug Substance and Pharmaceutical Dosage Form in the Presence of Its Degradation Products and Characterization of Main Degradation Products Based on LC-MS

Journal of Chromatographic Science ◽

10.1093/chromsci/bmz110 ◽

2019 ◽

Vol 58 (3) ◽

pp. 251-261

Author(s):

Hala E Zaazaa ◽

Rasha Abdel-Ghany ◽

M Abdelkawy ◽

Mahmoud Sayed

Keyword(s):

Dosage Form ◽

Degradation Products ◽

Hplc Method ◽

Drug Substance ◽

Design Parameters ◽

Pharmaceutical Dosage Form ◽

Stability Indicating ◽

Chromatographic Methods ◽

Hptlc Method

Abstract Two robust and selective stability-indicating chromatographic methods were developed and validated for the determination of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The HPLC method employed a Kromasil C18 (250 × 4.6,5 μm) column and a mobile phase of acetonitrile: 0.2% orthophosphoric acid (32:68 v/v) at a flow rate 2 mL/min and detection at 238 nm. The separation was performed in HPLC isocratic mode. The robustness of the suggested method was assessed using the Plackett–Burman design, parameters affecting system suitability were established and non-significant intervals for the significant parameters were considered. The HPTLC method employed Nano-SIL-20 UV254 HPTLC plates as adsorbent, ethyl acetate: toluene: acetic acid solution (4:4:0.5, v/v/v), as a developing solvent system and densitometric detection at 238 nm. Metolazone was exposed to different stress conditions, including acid and alkaline hydrolysis and oxidative and photolytic degradation. The main degradation products obtained have been characterized and interpreted based on LC-MS. The linearity of the suggested methods was proved in the concentration range of 20–75 μg/mL for the HPLC method and 100–900 ng/spot for the HPTLC method. The suggested methods were validated according to international conference on harmonization guidelines. These methods were successfully dedicated for the estimation of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The results of the suggested methods were evaluated and compared statistically with results obtained by an official method without finding any significant difference.

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Development and Validation of a Stability-Indicating RP-HPLC Method for Determination of Atomoxetine Hydrochloride in Tablets

Journal of AOAC International ◽

10.1093/jaoac/93.4.1207 ◽

2010 ◽

Vol 93 (4) ◽

pp. 1207-1214 ◽

Cited By ~ 4

Author(s):

Sejal K Patel ◽

Natvarlal J Patel

Keyword(s):

Degradation Products ◽

Hplc Method ◽

Stress Conditions ◽

Acid Base ◽

Photodiode Array Detection ◽

Stability Indicating ◽

Stability Indicating Method ◽

Rp Hplc ◽

Wet Heat

Abstract This paper describes the development of a stability-indicating RP-HPLC method for the determination of atomoxetine hydrochloride (ATX) in the presence of its degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of acid, base, oxidation, wet heat, dry heat, and photodegradation. In stability tests, the drug was susceptible to acid, base, oxidation, and dry and wet heat degradation. It was found to be stable under the photolytic conditions tested. The drug was successfully separated from the degradation products formed under stress conditions on a Phenomenex C18 column (250 4.6 mm id, 5 m particle size) by using acetonitrilemethanol0.032 M ammonium acetate (55 + 05 + 40, v/v/v) as the mobile phase at 1.0 mL/min and 40C. Photodiode array detection at 275 nm was used for quantitation after RP-HPLC over the concentration range of 0.55 g/mL with a mean recovery of 100.8 0.4 for ATX. Statistical analysis demonstrated that the method is repeatable, specific, and accurate for the estimation of ATX. Because the method effectively separates the drug from its degradation products, it can be used as a stability-indicating method.

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