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Sterol glycosides (SG) are known to cause filter blocking problems in biodiesel use. The extraction and quantitative analysis of SG is difficult due to its low problematic concentration and its compatibility with biodiesel. The purpose of this study is to develop a method to quantify SG in FAME and biodiesel using gas chromatography and other equipment found in laboratories performing routine biodiesel analyses. SG was isolated from FAME using n‐dodecane, acidification and cold soaking, followed by cold centrifugation at −8 to −15 °C. The solids obtained were further separated by phase partition with a Folch wash, followed by a final n‐dodecane rinse. This solution was analyzed by GC‐FID using the operating conditions outlined in ASTM D6584. A calibration curve for SG was produced and a first order fit gave a value of r2 = 0.992. Reproducibility tests were performed on soybean FAME and B100 canola biodiesel samples spiked with SG. The recovery of SG by the new method was found to be 99 % for soy FAME with a standard deviation of 0.7 and 100 % for B100 canola with a standard deviation of 3.5 %. The reproducibility based on two standard deviations of the predicted concentration for all 12 spiked samples studied in this work was 2.4 ppm.

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