Development of a simple and stability-indicating RP-HPLC method for determining olanzapine and related impurities generated in the preparative process

Development of a simple and stability-indicating RP-HPLC method for determining olanzapine and related impurities generated in the preparative process

Daoping Cui,^a   Yueqing Li,^a   Mingming Lian,^a   Feng Yang^b and  Qingwei Meng*^a  

*

Corresponding authors

^a

State Key Laboratory of Fine Chemicals, School of Pharmaceutical Science and Technology, Dalian University of Technology, No. 2 Linggong Road, Ganjingzi District, Dalian, P. R. China
E-mail: mengqw@dlut.edu.cn

^b

Merro Pharmaceutical Companies, No. 9 Yingsheng Road, Ganjingzi District, Dalian, P. R. China

Analyst, 2011,136, 3149-3156

DOI: 10.1039/C1AN15155Jhttp://pubs.rsc.org/en/content/articlelanding/2011/an/c1an15155j#!divAbstract

A simple and stability-indicating reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the determination of olanzapine (OLN) and related impurities in bulk drugs. Eight impurities were characterized respectively, and particularly a new process impurity from OLN synthesis was structurally confirmed as 1-(5-methylthionphen-2-yl)-1H-benzimidazol-2(3H)-one (Imp-7) by X-ray single crystal diffraction,MS, ¹H NMR, ¹³C NMR and HSQC. A mechanism of formation pathway for Imp-7 was proposed. Optimum separation for OLN and eight related impurities was carried out on an Agilent Octyldecyl silica column (TC-C₁₈, 4.6 mm × 250 mm, 5 μm) using a gradient HPLC method. The method was validated with respect to specificity, linearity, accuracy, precision, LOD and LOQ. Regression analysis showed good correlation (r² > 0.9985) between the investigated component concentrations and their peak areas within the test ranges for OLN and eight impurities. The repeatability and intermediate precision, expressed as RSD, were less than 1.74%. The proposed stability-indicating method was suitable for routine quality control anddrug analysis of OLN in bulk drugs.

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a State Key Laboratory of Fine Chemicals, School of Pharmaceutical Science and Technology, Dalian University of Technology, No. 2 Linggong Road, Ganjingzi District, Dalian, Liaoning Province, 116024, P. R. China. E-mail: mengqw@dlut.edu.cn














b Merro Pharmaceutical Companies, No. 9 Yingsheng Road, Ganjingzi District, Dalian, Liaoning Province, 116036, P. R. China

P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent.

P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent.

P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent.

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