A new approach to forced degradation studies using zolmitriptan tablets by a sensitive liquid chromatographic method (original) (raw)
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Chromatographia, 2013
Accurate, sensitive, and precise high performance thin layer chromatographic (HPTLC) methods were developed and validated for the determination of sumatriptan and zolmitriptan in presence of their degradation products. Sumatriptan was separated from its degradation products and analyzed on TLC silica gel 60 F 254 plates using chloroform-ethyl acetate-methanol-ammonia (4:3: 3:0.1, v/v) as a developing system followed by densitometric measurement of the bands at 228 nm. Zolmitriptan was determined using chloroform-ethyl acetate-methanolammonia (3:3:3:1, v/v) as a developing system followed by densitometric measurement at 222 nm. The methods were validated over a range of 0.5-4 lg/spot for sumatriptan and 0.5-3 lg/spot for zolmitriptan. The proposed methods were successfully applied for the determination of the studied drugs in bulk powder and in their pharmaceutical formulations.
A stability indicating LC method for zolmitriptan
Journal of Pharmaceutical and Biomedical Analysis, 2005
A gradient, reversed-phase liquid chromatographic (RP-LC) assay method was developed for the quantitative determination of zolmitriptan, used to treat severe migraine headaches. The developed method is also applicable for the related substances determination in bulk drugs. The chromatographic separation was achieved on a Waters X Terra RP18, 250 mm × 4.6 mm, 5 m column. The gradient LC method employs solutions A and B as mobile phase. The solution A contains a mixture of phosphate buffer pH 9.85:methanol:acetonitrile (70:20:10, v/v/v) and solution B contains a mixture of phosphate buffer, pH 9.85:acetonitrile (30:70). The flow rate was 1.0 ml/min and the detection wavelength was 225 nm. In the developed HPLC method, the resolution between zolmitriptan and its potential impurities, namely Imp-1, Imp-2 and Imp-3 was found to be greater than 3. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in alkaline medium and oxidative stress conditions. Degradation product formed during base hydrolysis was found to be Imp-3. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.
An Introduction to Forced degradation studies for drug substances and drug products
Journal of emerging technologies and innovative research, 2021
Forced degradation is basically degradation studies of may drug substances and drug products which are generally available in pharmaceutical industry. Forced degradation studies also known as stress testing studies, carried out to demonstrate developed stability indicating method by using high performance liquid chromatography i.e. HPLC. Forced degradation is a powerful tool used routinely in pharmaceutical development in order to develop stability indicating methods that lead to quality stability data and to understand the degradation pathways of the drug substances and drug products. This review discuss the trends in forced degradation studies. Forced degradation studies ensure appropriate stability of final pharmaceutical products in very early stages of pharmaceutical development.
The objective of the review article is to give detailed description and guidance of the forced degradation studies as per regulatory guidelines. Forced degradation study provide information about the degradation pathways and degradation products of the drug substance and helps in the elucidation of the structure of the degradation products. forced degradation study provide the chemical behaviour and chemical nature of the molecule which ultimately helps in the development of formulation during manufacturing and packaging specification, thus this review article provide knowledge of the current trends in performance of forced degradation study and establishing the analytical methods that helpful for development of stability indicating method. The stability of drug product and or drug substance is a critical parameter which may affect purity, potency and safety.
Current Trend in Performance of Forced Degradation Studies for Drug Substance and Drug Product’s
Journal of Drug Delivery and Therapeutics
The stability of a new drug substances and new drug products is a vital parameter which may affect purity, safety & potency. Changes in drug stability can threat patient safety by formation of toxic degradation products or deliver to lower dose than expected. Therefore it is to know the purity profile & behaviour of a drug substances under the various environmental condition. Forced Degradation studies show the chemical behavior of the molecule which in turn helps in the development of new formulation & package . Degradation study is required to the design of a regulatory compliant stability program for the both drug substances & products, and formalized as a regulatory requirement in ICH Guideline Q1A in 1993. Forced degradation studies (chemical and physical stress testing) of new chemical entities and drug product which is required to develop and demonstrate the specificity i.e stability indicating method. Forced degradation studies used to determination of the degradation pat...
A simple, specific, accurate and stability-indicating liquid chromatographic method has been developed for determination of sumatriptan in the presence of its alkaline degradation product and in pharmaceutical formulation. The analysis was carried out on Grace C18 (2.1 x 250 mm with 5 µm particle size) column with a mobile phase consisting of water (contains 0.1 % triethylamine, adjust pH to 6.5 by phosphoric acid): acetonitrile in the ratio (6 : 4, v/v). The detection was accomplished ûuorometrically setting the excitation wavelength at 225 nm and emission wavelength at 350 nm. The retention time was 4.1 min. and 5.2 min. for sumatriptan and its alkaline degradation, respectively, at flow rate 0.2 mL min -1 . The developed and validated method was successfully applied to the analysis of pharmaceutical formulation. The calibration curve was linear over the range 50-800 ng mL -1 . The LOD and LOQ values were found to be 16.6 and 50 ng mL -1 , respectively. Statistical analysis of the results has been carried out revealing high accuracy and good precision. A kinetic study of the degradation reaction was done and proved to follow pseudo-first order kinetics.