With 3-aminopropyltriethoxysilane (APTES) as coupling agent, poly(lactic acid) (PLA)/SiO2 hybrid material was prepared to produce poly(lactic acid)/SiO2 hybrid microspheres (PLAHs) with porous structure by the oil-in-water, single-emulsion solvent evaporation method. Field scanning electron microscopy results show that the PLAHs were porous microspheres about 20 pm in diameter. The holes in the PLAHs opened outside and were not complicated. A nitrogen adsorption-desorption experiment showed that the nitrogen adsorbed in the holes was easily desorbed, and the specific surface area of the PLAHs was calculated to be 6.87 m(2)/g according to the Brunauer-Emmett-Teller equation. Fourier transform infrared spectroscopy results show that PLA was amidated with APTES successfully and formed a kind of organic-inorganic hybrid material by hydrolysis and concondensation with tetraethoxysilane. Moreover, the molecular structure of the hybrid material was confirmed by X-ray photoelectron spectroscopy. Differential scanning calorimetry results show that the melting point of the PLAHs was higher than that of PLA by about 11.2 degrees C. These PLAHs may be used in the controlled release of drugs by the embedding of the drugs in the holes of the PLAHs, and the drug loading amount can be controlled by the size and number of holes in the PLAHs. (c) 2006 Wiley Periodicals, Inc.