Stability indicating LC method for rapid determination of related substances of O-desmethyl venlafaxine in active pharmaceutical ingredients and pharmaceutical formulations.
A simple, precise and accurate stability-indicating reversed phase-high performance liquid chromatography method was developed for the quantitative determination of O-desmethyl venlafaxine (ODV) and its related substances in active pharmaceutical ingredient and pharmaceutical formulation. The method was developed using YMC-pack ODS-A (150 × 4.6 mm, 3 μm) column with mobile phase containing a gradient mixture of solvents A and B. Solvent A contained a mixture of buffer and acetonitrile in the ratio of 85:15 (v/v). The buffer consisted of 10 mM potassium dihydrogen phosphate and 2 mM 1-octane sulfonic acid sodium salt (pH adjusted to 6.0 by using diluted potassium hydroxide solution). Solvent B contained a mixture of water and acetonitrile in the ratio of 20:80 (v/v). The eluted compounds were monitored at 230 nm. ODV and its six impurities were well separated within 14 min run time. It was subjected under the stress conditions of oxidative, acid, base, water, thermal and photolytic degradation. It was sensitive towards acidic, basic, oxidative and water stress conditions, stable in photolytic and thermal degradation conditions. The degradation products were well resolved from main peak and its impurities, the mass balance in each case was >99.0%, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to its specificity, linearity (correlation coefficient >0.9996), limit of detection, limit of quantification, accuracy (recovery range 97.1-103.2%), precision (% relative standard deviation ≤1.9%) and robustness.
Dr. Reddy's Laboratories Ltd., Active Pharmaceutical Ingredients, IPDO, Bachupally, Hyderabad 500072, AP, India Department of Chemistry, J. N. T. University, Kukatpally, Hyderabad 500072, AP, India visweswarark@drreddys.com vissu_karri@rediffmail.com.
Karri Visweswara
KV
Rao
Dr. Reddy's Laboratories Ltd., Active Pharmaceutical Ingredients, IPDO, Bachupally, Hyderabad 500072, AP, India.
Kesareddy Padmaja
KP
Reddy
Dr. Reddy's Laboratories Ltd., Active Pharmaceutical Ingredients, IPDO, Bachupally, Hyderabad 500072, AP, India.
Yelavarthi Ravindra
YR
Kumar
D056148:Chromatography, Reverse-Phase / Q000379:methods*; D003511:Cyclohexanols / Q000032:analysis* / Q000737:chemistry*; D000069468:Desvenlafaxine Succinate; D004340:Drug Contamination; D004355:Drug Stability; D057230:Limit of Detection; D016014:Linear Models; D015203:Reproducibility of Results
D003511:Cyclohexanols; D000069468:Desvenlafaxine Succinate