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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 &amp;gt;0.999, relative standard deviation (RSD) of the slope &amp;lt;1.3, and RSD of the response factors &amp;lt;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

Gas Chromatographic Determination of High Molecular Weight Alcohols from Policosanol in Omega-3 Fish Oil by Acylation with Acetyl Chloride