Our recent studies have shown that certain citrus limonoids protect from colon cancer based on cell and animal studies. Animal studies also suggest that citrus juice protects from osteoporosis. To understand the structure–function relationship through animal studies requires a large amount of purified limonoids. Since certain limonoids are present in low concentration, it is a challenge to obtain the required quantity of different limonoids. In this context, we report the purification of limonin 17-ß-D glucopyranosides (LG), and deacetylnomilinic acid 17-ß-D glucopyranoside (DNAG). However, DNAG was isolated in relatively large amount from sour orange (Citrus aurantium L.) seeds. Defatted seed powder was extracted with methanol and purified using column chromatography to obtain multigrams of DNAG. While LG was found in lower concentration, a large concentration of hesperidin was also purified in this process. This project is based upon work supported by the USDA-CSREES under Agreement USDA IFAFS #2001 52102 02294 and USDA #2005-34402-14401 “Designing Foods for Health” through the Vegetable & Fruit Improvement Center.