Static headspace gas chromatographic method for quantitative determination of residual solvents in pharmaceutical drug substances according to European Pharmacopoeia requirements

被引：55

作者：

Otero, R ^{[1
]}

Carrera, G ^{[1
]}

Dulsat, JF ^{[1
]}

Fábregas, JL ^{[1
]}

Claramunt, J ^{[1
]}

机构：

[1] Res Ctr St Feliu Llobregat, Anal R&D Dept, Barcelona 08980, Spain

来源：

JOURNAL OF CHROMATOGRAPHY A | 2004年 / 1057卷 / 1-2期

关键词：

validation; headspace analysis; standard addition; pharmaceutical drug substance; residual solvents; European pharmacopoeia;

D O I：

10.1016/j.chroma.2004.09.023

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

A static headspace (HS) gas chromatographic method for quantitative determination of residual solvents in a drug substance has been developed according to European Pharmacopoeia general procedure. A water-dimethylformamide mixture is proposed as sample solvent to obtain good sensitivity and recovery. The standard addition technique with internal standard quantitation was used for ethanol, tetrahydrofuran and toluene determination. Validation was performed within the requirements of ICH validation guidelines Q2A and Q2B. Selectivity was tested for 36 solvents, and system suitability requirements described in the European Pharmacopoeia were checked. Limits of detection and quantitation, precision, linearity, accuracy, intermediate precision and robustness were determined, and excellent results were obtained. (C) 2004 Elsevier B.V. All rights reserved.

引用

页码：193 / 201

页数：9

共 17 条

[11] RESIDUAL SOLVENT ANALYSIS BY HEADSPACE GAS-CHROMATOGRAPHY [J].

KUMAR, N ;

GOW, JG .

JOURNAL OF CHROMATOGRAPHY A, 1994, 667 (1-2) :235-240

[12] Artefact formation in the determination of residual solvents according to a method of the European Pharmacopeia [J].

Lee, CR ;

van Dau, CN ;

Krstulovic, AM .

INTERNATIONAL JOURNAL OF PHARMACEUTICS, 2000, 195 (1-2) :159-169

[13] A capillary gas chromatographic procedure for the analysis of nine common residual solvents in water-insoluble bulk pharmaceuticals [J].

Li, QC ;

Cohen, KA ;

Zhuang, G .

JOURNAL OF CHROMATOGRAPHIC SCIENCE, 1998, 36 (03) :119-124

[14]

Miller J.N., 2000, STAT CHEMOMETRICS AN

[15] Comparison of quantitative analytical methods in headspace gas chromatography of residual solvents [J].

Naddaf, A ;

Balla, J .

CHROMATOGRAPHIA, 2000, 51 (1) :S241-S248

[16]

*US PHARM CONV, 2003, ORG VOL IMP METH 4 5, P2078

[17] Residual solvents in pharmaceutical products: Acceptable limits, influences on physicochemical properties, analytical methods and documented values [J].

Witschi, C ;

Doelker, E .

EUROPEAN JOURNAL OF PHARMACEUTICS AND BIOPHARMACEUTICS, 1997, 43 (03) :215-242

← 1 2 →