Background:To understand the degradation behavior of diacerein and to develop a simple, rapid, sensitive, and validated RP-HPLC method for the determination of diacerein, in the presence of its degradation products.Materials and Methods:An accurate, sensitive, precise, rapid, and isocratic reversed-phase high-performance liquid chromatography (RP-HPLC) method, equipped with a photo-diode array (PDA) detector for analysis of diacerein in the bulk drug has been developed and validated. The best separation was achieved on a 250 mm × 4.6 mm i.d., 5-μm particle, RP C18 column with 50 : 50 (v/v) of water (pH adjusted to 2.9 with orthophosphoric acid) : acetonitrile as the mobile phase, at a flow rate of 1.0 ml/minute. The detection wavelength was set at 257 nm.Results:The response was a linear function of concentration over the range of 0.50 – 20 μg/ml (r = 0.999) and the limits of detection and quantitation were 0.1 μg/ml and 0.50 μg/ml, respectively. The method was validated in accordance with the International Conference on Harmonization (ICH) guidelines. The drug was subjected to oxidative, hydrolytic, photolytic, and thermal stress. The drug decomposed under alkaline hydrolytic stress conditions and also on thermal degradation and photolysis. It was stable on acid hydrolysis and oxidation. The degradation products produced as a result of this stress did not interfere with the detection of diacerein, and the assay could thus be regarded as stability-indicating.Conclusion:The method was suitable for application in the analysis of formulations of diacerein in quality-control laboratories, because it was simple and rapid, with good accuracy and precision.
drug efavirenz is still not ofÞ cial in USP or BP, and there are no ofÞ cial HPTLC method reported for analysis of efavirenz from bulk drugs. Thus, an appropriate analytical procedure for the quantitative determination of efavirenz from bulk drugs is of considerable importance. Keeping this objective in mind an attempt has been made INTRODUCTION Efavirenz [Figure 1], (4S)-6-chloro-4-(cyclopropylethynyl)-1,4-dihydro-4-(triß uoromethyl)-2H-3, 1-benzoxazin-2-one, is a non-nucleoside reverse transcriptase (RT) inhibitor of human immunodeÞ ciency virus type 1 (HIV-1). [1,2] Efavirenz activity is mediated predominantly by noncompetitive inhibition of HIV-1 RT. HIV-2 RT and human cellular DNA polymerases alpha, beta, gamma, and delta are not inhibited by efavirenz. [3] The literature survey reveals that there are analytical methods available for determination of efavirenz from biological matrices, [4-9] bulk drug, and dosage forms, [10,11] and analytical methods for determination of efavirenz with combination of other antiviral drugs. [12-35] However, there is no reported HPTLC method for the analysis of efavirenz. The literature survey further revealed that the Pharm Analysis
The concept of Quality by design (QbD) has recently gained importance in the area of analytical method development and involves understanding of the critical factors and their interaction effects by a desired set of experiments. So, the present work describes the development of Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method by QbD approach using Design of Experiments and subsequent validation for analysis of Vildagliptin in bulk drug and its pharmaceutical formulation. An efficient experimental design based on systematic scouting of all three key components of the RP‐HPLC method (Buffer pH, Organic Phase-% acetonitrile, Organic Modifier-Methanol) is presented. The significance and interaction effects of these parameters on the response variables (Retention time and tailing factor) were evaluated through statistical analysis tools like Analysis of Variance (ANOVA) and plots which revealed the final chromatographic conditions of the method. The developed method was validated and Forced degradation studies were also carried out in order to determine the stability-indicating nature of the method. The chromatographic separation was achieved on Jasco CrestPack RP C18 (250 × 4.6 mm, 5μ) column using Buffer (pH 6): Acetonitrile: Methanol (70:10:20 v/v) as mobile phase and detection was done using Photo-Diode Array (PDA) detector at 210 nm. The developed method of Vildagliptin is linear over a range of 5-15μg/ml having correlation coefficient R2 value as 0.999. The %RSD for precision and accuracy of the method was found to be less than 2%. Forced Degradation studies revealed that the method was found to be stability-indicating. The results showed that the proposed method is suitable for the precise and accurate determination of Vildagliptin in bulk and its formulation.
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