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Pushpalatha P.,Central Forensic Science Laboratory | Sarin R.,Central Forensic Science Laboratory | Idris M.,Central Forensic Science Laboratory | Rao M.,Osmania University | And 2 more authors.
Journal of Planar Chromatography - Modern TLC | Year: 2013

A rapid, sensitive, and specific high-performance thin-layer chromatographic (HPTLC) method was developed and validated for quantitative determination of free duloxetine (DLX) in human serum. Densitometric analysis of free DLX was carried out at 235 nm after simple liquid-liquid extraction. The method uses thinlayer chromatography (TLC) aluminum plates pre-coated with silica gel G 60 F254 as stationary phase and acetone-benzene- triethylamine (5:4.5:0.5, v/v) as mobile phase for the separation of free DLX from serum constituencies. The calibration curve was linear (r2 = 0.980) in the tested range of 35-140 ng spot-1 with a limit of quantification and detection of 35 and 10 ng spot-1 with the recovery of free DLX in serum ranges from 92.86 to 97.58%. Intra- and inter-day precision (% RSD) values were â‰1.83% and â‰5.66%, respectively. Analysis of free DLX from human serum was successfully performed without interference from endogenous materials and some of the other common drugs of abuse. The method's ability to quantify free DLX with precision, accuracy, and sensitivity makes it useful in forensic examination.

Kumar N.,IPDO Dr. Reddys Laboratories Ltd. | Kumar N.,Vellore Institute of Technology | Sangeetha D.,Vellore Institute of Technology | Goyal R.,IPDO Dr. Reddys Laboratories Ltd. | Reddy P.,IPDO Dr. Reddys Laboratories Ltd.
Acta Chromatographica | Year: 2013

A simple, selective, and stability-indicating reverse phase liquid chromatographic method has been developed and validated for the simultaneous determination of impurities and forced degradation products of quetiapine fumarate. The chromatographic separation was achieved on Inertsil-3 C8, 150 mm × 4.6 mm, 5 μm column at 35 C with UV detection at 217 nm using gradient mobile phase at a flow rate of 1.0 mL/min. Mobile phase A contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 80:20 (v/v), respectively, and mobile phase B contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 20:80 (v/v), respectively. The drug product was subjected to the stress conditions of oxidative, hydrolysis (acid and base), hydrolytic, thermal, and photolytic degradation. Quetiapine fumarate was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from main peak and its impurities. The mass balance was found to be in the range of 96.6-102.2% in all the stressed conditions, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.

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