Development and validation of a high-performance thin-layer chromatographic method for the determination of biomarker β-amyrin in the leaves of differentFicusspecies

To develop a simple, fast, specific, precise and accurate High Performance Thin Layer Chromatographic method (HPTLC) for the determination of Voglibose in bulk and their dosage forms. The chromatographic separation was achieved on precoated silica gel 60F254 aluminum plates using a combination of acetonitrile: methanol: ammonia (15:4:0.1 % V/V/V) as mobile phase and densitometric evaluation of spots was carried out at 284 nm using Camag TLC scanner III with CATS 1.3.4 version software. The experimental parameters like band size of the chamber saturation time, spot application, slit width, solvent front migration, etc. were studied critically and evolved optimized conditions. The drug was well resolved satisfactorily with Rf value 0.66±0.03. The repeatability and accuracy of the optimized method were ascertained by evaluating various validation parameters like linearity (100 to 450 ng/spot), precision (intra-day % RSD 0.21 to 0.74, inter-day % RSD 0.21 to 0.29), accuracy (99.8% to 101.2%, % RSD below 1%), and specificity according to ICH guidelines. The limits of detection and quantification were 40 ng/spot and 100 ng/spot respectively. The developed HPTLC method was faster and cost effective quantitative control for routine analysis of Voglibose in bulk and its formulations.

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A NEW HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD DEVELOPMENT AND VALIDATION OF DAPAGLIFLOZIN IN BULK AND TABLET DOSAGE FORM

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2019v11i8.34339 ◽

2019 ◽

pp. 58-63

Author(s):

B. V. SUMA ◽

DEVESWARAN R. ◽

PREMNATH SHENOY

Keyword(s):

Thin Layer ◽

High Performance ◽

Dosage Form ◽

Chromatographic Method ◽

Method Development ◽

Retention Factor ◽

Accurate Analysis ◽

Development And Validation ◽

Tablet Dosage

ABSTRACT Objective: To develop a new simple, selective and precise high-performance thin layer chromatographic method for determination of Dapagliflozin (DAPA) in bulk and tablet dosage form Methods: The present study describes development and validation of High performance thin layer chromatographic method for DAPA. The chromatographic separation was carried out on Merck precoated silica gel aluminium plate 60 F254 using Chloroform: Methanol (9:1v/v) as mobile phase. Quantitative determination of drug was carried out by densitometric scanning of plates at 223 nm using Camag TLC Scanner. Results: The chromatographic condition shows compact band with the retention factor for dapaglifloxin as 0.21 ± 0.004. The method was validated as per ICH guidelines for linearity, accuracy, precision and robustness. Response was found to be linear in the concentration range of 400 ng/ band to 1200 ng/band with linear regression value of 0.9953 with respect to peak area and concentration value The LOD and LOQ was found to be 1.2083 ng/band and 3.6616ng/ band. The percentage assay was found to be 100±0.05. Conclusion: This method under statistical analysis proved a selective, repeatable and accurate analysis of the drug. This method can be used for quantitative analysis of dapaglifloxin in the bulk drug and in tablet.

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