In　this　work,　the　chemiluminescence　analysis　method　was　used　to　detect　the　free　radical　during　sonodynamic　process.　MCLA,　which　can　specifically　react　with　singlet　oxygen　(1O2)　or　superoxide　anion　to　emit　photon,　was　used　to　detect　free　radical　formation　in　the　sonosensitization　of　metallophthalocyanine　in　real　time.　The　ultrasound-induced　chemiluminescence　of　MCLA　enhanced　by　sulfonated　phthalocyanines　Nickel　did　not　show　the　expected　structure-activity　relationship　which　was　well　known　as　type　II　mechanism　for　the　photodynamic　therapy　related　to　singlet　oxygen　production.　The　results　showed　that　free　radical　are　involved　in　the　sonosensitization,　and　the　catalytic　performance　of　NiPcS4　was　the　main　reason　for　the　increase　of　SCL.　©　2011　Elsevier　B.V.　All　rights　reserved.