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Published on:August 2021
Indian Journal of Pharmaceutical Education and Research, 2021; 55(3):904-915
Original Article | doi:10.5530/ijper.55.3.165

Chemometric Assisted Development and Validation of a Stability-indicating LC Method for Determination of Related Substances in Haloperidol Decanoate Injection

Authors and affiliation (s):

Sudheer Kolla Babu1,2*, Madhusudhan Vallabhaneni Rao1, Srinivasa Puttagunta Babu3, Murthy Veera Venkata Satyanarayana Chakka2

1Vignan’s Foundation for Science, Technology and Research University, Vadlamudi, Guntur, Andhra Pradesh, INDIA.

2Department of Analytical Research and Development, Formulations, GVK Bio Sciences Pvt. Ltd., Mallapur, Hyderabad, Telanagana, INDIA.

3Department of Pharmaceutics, Vignan Pharmacy College, JNTU-Kakinada, Vadlamudi, Guntur, Andhra Pradesh, INDIA.


Aim: Haloperidol decanoate injection is a phenyl butyl piperadine derivative with antipsychotic, neuroleptic, antiemetic effects and has multiple related substances as process and degradant impurities. Objectives: This study focuses on chemometric assisted liquid chromatographic approach to develop a stability indicating impurity profile of Haloperidol decanoate injection. Methodology: Dual experimental designs (combined mixture I-optimal design and response surface historical data design) were employed to resolve all thirteen known impurities of Haloperidol decanoate. Chromatographic separation was achieved on a Hypersil BDS C18 (100 x 4.0 mm) 3-μm column to attain separation of related compounds. Results: The optimum conditions for the chromatographic system resulted in a mobile phase consisting of tetra butyl ammonium hydrogen sulphate/ 1-decane Sulphonate sodium buffer solution and acetonitrile with linear gradient elution at a flow rate of 1.4 mL/min. Selectivity, forced degradation, linearity, accuracy and precision were demonstrated in a range of 0.75-30.0 μg/mL. Conclusion: The optimized method was able to resolve the ghost peak observed because of gradient change of mobile phase and is able to separate both polar and non-polar impurities within 60 min, in single method, with resolution of more than 2.0 between adjacent impurities. The inter-day precision for all impurities and haloperidol decanoate were evaluated and found to have a % RSD of less than 10.

Key words: Design of Experiments, Haloperidol decanoate Injection, Stability indicating method, DoE aided chromatographic method development, Artifact optimization.



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The Official Journal of Association of Pharmaceutical Teachers of India (APTI)
(Registered under Registration of Societies Act XXI of 1860 No. 122 of 1966-1967, Lucknow)

Indian Journal of Pharmaceutical Education and Research (IJPER) [ISSN-0019-5464] is the official journal of Association of Pharmaceutical Teachers of India (APTI) and is being published since 1967.


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