Observations of VOCs concentration were conducted at a litchi plantation in the Pearl River Delta in July 2008 and February-March 2009 respectively. VOCs fluxes were estimated based on the relationship of flux-gradient and REA method using the VOCs concentration data. Statistical evidence indicates that the major emission matter is isoprene with a typical daytime mean flux 0.932 nmol/(m2?s) in the growing season over the litchi plantation. While in the non growing season, the flux is negligible. This study provides a reliable reference not only for emission rates for litchi and manmade plantation, but also for usage of micrometeorological methods to measure VOCs fluxes.