High ultrasonic-assisted extraction technology (INEFU) was employed to extract the active components from natural materials (green coffee beans, Citrus madurensis, Centella asiatica, Laminaria Japonica). The extraction conditions were optimized by a response surface method and Box-Behnken design. The active component yields were obtained under the optimum parameters: ultrasound power (1800 watts), ultrasonication time, and particle size. After INEFU of natural materials (green coffee beans, Citrus madurensis, Centella asiatica and Laminaria Japonica) the products were analyzed with high performance liquid chromatography (HPLC). HPLC analysis showed that the four natural materials were composed of different combinations of vitamin C, polyphenols, chlorogenic acid, caffein, caffeic acid, asiaticoside and alginic acid. In addition, the INEFU results showed that natural materials can yield more active components during a simulated extraction process.