Document Detail


Evaluation of a capillary gas chromatographic impurity test procedure for 4-hexylaniline.
MedLine Citation:
PMID:  15975246     Owner:  NLM     Status:  PubMed-not-MEDLINE    
Abstract/OtherAbstract:
A capillary gas chromatographic test procedure for the detection and quantitation of impurities in the bulk intermediate, 4-hexylaniline, is evaluated and found to be accurate and precise. 4-Hexylaniline is dissolved in methanol and chromatographed isothermally at a temperature of 195 degrees C on a 60-m x 0.32-mm 85% polyethylene glycol-15% dimethylsilicone blend (DX-4) film column. A flame ionization detector is used, and the impurities in the parent compound are estimated from peak areas on a percent basis compared with the area of the parent peak in the chromatogram. Response factors are determined for the known impurities. Validation of this test method includes a recovery study of known impurity spiked samples fortified in the range of 0.1-1% (w/w). A repeatability study is performed, consisting of the analysis of two different synthetic batch lots of 4-hexylaniline analyzed over three experimental run days using two chromatographic columns of different manufacturing lots. These data and other aspects of this test procedure are discussed.
Authors:
C B'Hymer
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Publication Detail:
Type:  Journal Article    
Journal Detail:
Title:  Journal of chromatographic science     Volume:  43     ISSN:  0021-9665     ISO Abbreviation:  J Chromatogr Sci     Publication Date:    2005 May-Jun
Date Detail:
Created Date:  2005-06-24     Completed Date:  2005-09-27     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  0173225     Medline TA:  J Chromatogr Sci     Country:  United States    
Other Details:
Languages:  eng     Pagination:  267-70     Citation Subset:  -    
Affiliation:
University of Cincinnati, Mail Location 0172, Cincinnati, OH 45221-0172, USA. bhymerc@email.uc.edu
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