A simple, robust, precise, and accurate stability-indicating
reverse-phase high-performance liquid chromatographic (RP-HPLC) method was
successfully developed and validated for the simultaneous estimation of
Duloxetine (DLU) and Methylcobalamin (MCB) in their combined pharmaceutical
dosage form. The chromatographic analysis was performed on an Inertsil C18
column with dimensions 4.6 × 250 mm and particle size 5 µm, utilising an
isocratic elution technique. The mobile phase consisted of a phosphate buffer adjusted
to pH 4.5, which facilitated adequate separation of the analytes. The flow rate
of the mobile phase was maintained at 1.0 mL/min, and detection of the eluted
components was carried out at a wavelength of 255.0 nm using a UV detector.
Under the optimised chromatographic conditions, Duloxetine and Methylcobalamin
were eluted at retention times of approximately 5.32 minutes and 3.59 minutes,
respectively. The developed method showed excellent linearity over the
concentration ranges of 20–120 µg/mL for Duloxetine and 10–60 µg/mL for
Methylcobalamin. The correlation coefficients (r²) for both analytes were found
to be 0.999, indicating a strong linear relationship between peak area and
concentration within the specified ranges. Method accuracy was assessed by
recovery studies, which demonstrated mean percentage recoveries of 99.68% for
Duloxetine and 100.3% for Methylcobalamin, confirming the accuracy of the
method. The relative standard deviation (RSD) values for both analytes in
recovery studies were found to be not more than 2% (NMT 2%), reflecting high
precision and reproducibility of the method. Precision was further evaluated by
conducting intra-day and inter-day studies, both of which showed RSD values
within acceptable limits (NMT 2%) for both drugs, supporting the reliability
and repeatability of the method over different days and time intervals.
The developed RP-HPLC method was validated as per the
International Council for Harmonisation (ICH) guidelines, ensuring that all
critical parameters, including specificity, linearity, accuracy, precision,
robustness, and system suitability, were thoroughly assessed and met the
established acceptance criteria. The proposed method is therefore considered
suitable for the routine quality control and stability analysis of Duloxetine
and Methylcobalamin in their combined dosage forms.
Author(s) Details
Kandiboti Lavanya
Department of Pharmaceutical Analysis, Sir C. R. Reddy College of
Pharmaceutical Sciences, Eluru, Andhra Pradesh, India.
V. Anitha Kumari
Department of Pharmaceutical Analysis, Sir C. R. Reddy College of
Pharmaceutical Sciences, Eluru, Andhra Pradesh, India.
V. Srinivasa Rao
Department of Pharmacy Practice, Lydia College of Pharmacy, Ravulapalem,
Andhra Pradesh, India.
Please see the book here:- https://doi.org/10.9734/bpi/psnid/v7/5962
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