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Development and validation of chiral LC method for the enantiomeric separation of duloxetine on amylose based stationary phase.
J Chromatogr Sci. 2008 Oct; 46(9):772-6.JC

Abstract

A simple, rapid, and robust liquid chromatography method was developed and validated for the enantiomeric separation of duloxetine in bulk drug substance. The enantiomers of duloxetine were resolved on a Chiralpak AD-H (amylose based stationary phase) column using a mobile phase consisting of n-hexane-ethanol-diethyl amine (80:20:0.2, v/v/v) at a flow rate of 1.0 mL/min. The resolution between the enantiomers was found to be not less than 2.8 in optimized method. The presence of diethyl amine in the mobile phase played an important role in enhancing chromatographic efficiency and resolution between the enantiomers. The developed method was extensively validated and proved to be robust. The calibration curve for (R)-enantiomer showed excellent linearity over the concentration range of 750 ng/mL (LOQ) to 7500 ng/mL. The limit of detection and quantitation for (R)-enantiomer were 250 and 750 ng/mL, respectively. The percentage recovery of the (R)-enantiomer ranged between 98.3% to 101.05% in bulk drug samples of duloxetine. The proposed method was found to be suitable and accurate for quantitative determination of (R)-enantiomer in bulk drug substance.

Authors+Show Affiliations

Department of Chemical Technology, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad-431004 (MS), India.No affiliation info available

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

19007477

Citation

Rane, V P., and D B. Shinde. "Development and Validation of Chiral LC Method for the Enantiomeric Separation of Duloxetine On Amylose Based Stationary Phase." Journal of Chromatographic Science, vol. 46, no. 9, 2008, pp. 772-6.
Rane VP, Shinde DB. Development and validation of chiral LC method for the enantiomeric separation of duloxetine on amylose based stationary phase. J Chromatogr Sci. 2008;46(9):772-6.
Rane, V. P., & Shinde, D. B. (2008). Development and validation of chiral LC method for the enantiomeric separation of duloxetine on amylose based stationary phase. Journal of Chromatographic Science, 46(9), 772-6.
Rane VP, Shinde DB. Development and Validation of Chiral LC Method for the Enantiomeric Separation of Duloxetine On Amylose Based Stationary Phase. J Chromatogr Sci. 2008;46(9):772-6. PubMed PMID: 19007477.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and validation of chiral LC method for the enantiomeric separation of duloxetine on amylose based stationary phase. AU - Rane,V P, AU - Shinde,D B, PY - 2008/11/15/pubmed PY - 2008/12/17/medline PY - 2008/11/15/entrez SP - 772 EP - 6 JF - Journal of chromatographic science JO - J Chromatogr Sci VL - 46 IS - 9 N2 - A simple, rapid, and robust liquid chromatography method was developed and validated for the enantiomeric separation of duloxetine in bulk drug substance. The enantiomers of duloxetine were resolved on a Chiralpak AD-H (amylose based stationary phase) column using a mobile phase consisting of n-hexane-ethanol-diethyl amine (80:20:0.2, v/v/v) at a flow rate of 1.0 mL/min. The resolution between the enantiomers was found to be not less than 2.8 in optimized method. The presence of diethyl amine in the mobile phase played an important role in enhancing chromatographic efficiency and resolution between the enantiomers. The developed method was extensively validated and proved to be robust. The calibration curve for (R)-enantiomer showed excellent linearity over the concentration range of 750 ng/mL (LOQ) to 7500 ng/mL. The limit of detection and quantitation for (R)-enantiomer were 250 and 750 ng/mL, respectively. The percentage recovery of the (R)-enantiomer ranged between 98.3% to 101.05% in bulk drug samples of duloxetine. The proposed method was found to be suitable and accurate for quantitative determination of (R)-enantiomer in bulk drug substance. SN - 0021-9665 UR - https://www.unboundmedicine.com/medline/citation/19007477/Development_and_validation_of_chiral_LC_method_for_the_enantiomeric_separation_of_duloxetine_on_amylose_based_stationary_phase_ L2 - https://academic.oup.com/chromsci/article-lookup/doi/10.1093/chromsci/46.9.772 DB - PRIME DP - Unbound Medicine ER -