Isolation and characterisation of process-related impurities in rofecoxib

被引：12

作者：

Reddy, KVSRK

Babu, JM

Dubey, PK

Sekhar, BC

Reddy, GO

Vyas, K

机构：

[1] Dr Reddys Res Fdn, Dept Analyt Res, Hyderabad 500050, Andhra Pradesh, India

[2] JNT Univ, Dept Chem, Hyderabad 500872, Andhra Pradesh, India

[3] Dr Reddys Labs Ltd, Technol Dev Ctr, Hyderabad 500050, Andhra Pradesh, India

来源：

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2002年 / 29卷 / 1-2期

关键词：

rofecoxib; impurities; spectroscopy; identification and characterisation;

D O I：

10.1016/S0731-7085(02)00034-1

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

Two unknown impurities in rofiecoxib bulk drug at levels below 0.1% were detected by a simple isocratic reverse phase high performance liquid chromatography (HPLC). These impurities were isolated from crude sample of rofecoxib using reverse phase preparative HPLC. H-1, C-13 and Mass spectroscopic investigations revealed the structures of the impurities as 4-[4-(methylsulphonyl)phenyll-3-phenyl-5-hydroxyfuran-2-one (1) and 4-[4-(methylsulphonyl)phenyl]-3-phenyl-2,5-furandione (11), respectively. These structures were further confirmed by prepared synthetic standards of the impurities. The tentative mechanism for the formation of these impurities was discussed. (C) 2002 Elsevier Science B.V. All rights reserved.

引用

页码：355 / 360

页数：6

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