Gas Chromatographic Determination of High Molecular Weight Alcohols from Policosanol in Omega-3 Fish Oil by Acylation with Acetyl Chloride
Abstract:A new validated gas chromatographic (GC) method using acetyl chloride as a derivatizing agent for determining policosanol's high molecular weight alcohols (policosanol's fatty alcohols; PFAs) in fish oil (FO) is described. Before derivatizing the alcohols, FO was subjected to a methylation reaction, and then the PFAs were isolated in a chloroform fraction by silica gel by column liquid chromatography. GC analysis was performed using a BPX-5 wide-bore column and 1-eicosanol as an internal standard. Validation assays applied to the method proved noninterference by a very complex mixture of the FO with PFAs, even for samples subjected to stress conditions. Good linearity [correlation coefficient >0.999, relative standard deviation (RSD) of the slope <1.3, and RSD of the response factors <1.9 with no bias] and accuracy (average recovery from 100.6 to 102.2) over a range of 28142 of the nominal concentration were obtained. Within-day and intermediate precisions at the nominal dose (100) were 1.7 and 2.9, respectively. The method was successfully used to identify and quantitate the PFAs in FO.
Document Type: Research Article
Affiliations: Center of Natural Products, National Center for Scientific Research, Cubanacn, Playa, PO Box 6414, Havana City, Cuba.
Publication date: September 1, 2008
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- The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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