Dr. Reddys Laboratories Ltd. andhra Pradesh State

andhra Pradesh, India

Dr. Reddys Laboratories Ltd. andhra Pradesh State

andhra Pradesh, India
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Raghu N.S.,Dr. Reddys Laboratories Ltd. andhra Pradesh State | Raghu N.S.,Andhra University | Reddy Y.R.,Andhra University | Naresh V.,Dr. Reddys Laboratories Ltd. andhra Pradesh State | Rao V.S.,Andhra University
Journal of Liquid Chromatography and Related Technologies | Year: 2011

A simple, rapid, accurate, robust, sensitive, and stability-indicating reversed-phase high-performance liquid chromatographic (RP-HPLC) analytical method has been developed for the separations of related impurities and degradants of topotecan in topotecan injection. Forced degradation studies performed on topotecan injection formulation revealed that the compound (topotecan) is extremely susceptible to all hydrolytic, oxidation, light exposure, and thermal stress. The method was tested in the presence of commonly used formulation excipients such as mannitol and tartaric acid. Separation of topotecan from its degradation products and three related impurities (Imp-A, Imp-B, Imp-C) as process impurities was achieved on ACE® C18, 150 × 4.6 mm i.d, 3 μm, stainless steel analytical column using a gradient elution. The elution of impurities employed multi-step gradient programmed mobile phase consisting of 0.02M ammonium acetate (pH, 4.2) as mobile phase-A and a mixture of methanol and isopropyl alcohol in the ratio of 750:250 (v/v), respectively, as mobile phase-B. The mobile phase flow rate was maintained at 0.8 mL min-1. The column eluent was monitored at 267nm. The column oven temperature was 25°C. The same method was also extended to LC-MS with the same gradient conditions used to identify the degradation products observed under forced degradation studies. The method was validated according to FDA, USP (general chapter 1225), and ICH guidelines, and statistical analysis of the data proved to be suitable for stability testing at quality control. The linearity of the proposed method for all the aforementioned related impurities and topotecan was investigated in the range of LOQ to 4.9 μg mL-1, respectively. The method was shown to separate topotecan well from the degradants and commonly used excipients. The specificity of the method was established through peak purity testing using a photodiode array detector. Copyright © Taylor & Francis Group, LLC.


Raghu N.S.,Dr. Reddys Laboratories Ltd. andhra Pradesh State | Raghu N.S.,Andhra University
Journal of Liquid Chromatography and Related Technologies | Year: 2011

A new ion exchange high performance liquid chromatographic (IEC) method has been developed and validated for quantitative determination of Zoledronic acid in pharmaceutical injection dosage form. Complete separation was achieved for the parent compound Zoledronic acid, the impurities and excipients in an overall analytical run time of approximately 20 minutes. The proposed chromatographic conditions employed an isocratic elution of mobile phase at constant eluent flow rate of 0.7mLmin-1 and by using a new generation Allsep anion exchange column. A UV-Vis detector set at 215nm was used to monitor the eluate. The 100% aqueous mobile phase consisted of only diluted formic acid without any ion-pair substance. The drug product was subjected to oxidation, hydrolysis, photo-stability, and heat to apply the stress conditions. The method was found to be linear over the concentrations range from 0.200 to 1.200mgmL-1(25% to 150% of Zoledronic acid concentration). The newly developed method has the requisite accuracy, selectivity and precision to assay Zoledronic acid in commercial pharmaceutical injection dosage form. © Copyright © 2011 Taylor & Francis Group, LLC.

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