An efficient and inexpensive semi-micro liquid–liquid extraction method has been developed for simultaneous clean-up and extraction of vitamin A and vitamin E in infant milk formula samples. After saponification of milk samples, extraction procedure was done in a 5-mL volumetric flask. 4.5 mL of saponified sample solution was added to the volumetric flask, and then 300 lL of organic solvent was added slowly to the surface of the saponified solution in the neck of the flask by a gas tight micro syringe. The mixture was agitated during the extraction time. After the extraction time a prescribed amount of organic phase was withdrawn, evaporated and reconstituted with methanol and finally was injected into the HPLC system for analysis. The proposed method provided good reproducibility (3.9–5.1%), good linearity (0.006–80 lgmL
1 for vitamin A and 0.1–400 lgmL
1for vitamin E), low detection limits (0.003 lgmL
1 for vitamin A and 0.08 lgmL
1 for vitamin E), and was a simple, low cost, efficient, and easy handling technique for determination of vitamin A and E according to the results obtained. Furthermore, using monolithic column has the advantage of decreasing the total time of analysis.

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