First like always grind the samples in liquid nitrogen. For long-chain-fats you need chloroform or dichlormethane definitely in the extraction liquid. chloroform 2:1 Methanol is still the best method to extract lipids completely. No other organic solvent can beat chloroform because it's breaking down the structure of the tissue. For MS dont use any plastik with chloroform. Work only with glasware, PTFE or metal. Then lipid fractionation with HPLC, TLC or SPE (Kaluzny) . For protein others may talk...