Supercritical fluid extraction with methanol-modified CO(2) was used to extract glycosides from grapes. An optimization design involving 12 extraction variables was applied to achieve quantitative recoveries. The most important factor was the amount of organic modifier, a consequence of the high degree of glycoside polarity. By the proposed method, the total time of analysis can be decreased relative to that required for more conventional extractions. The full method can also be automated.