The automated, miniaturized, and solvent-free sample preparation method for determination of organic compounds in a solute-type combination matrix is discussed. The various characteristics of sample preparation methods include automation, miniaturization, and online and solventless sample preparation with high-throughput capability. These characteristics provide intelligent autosamples enabling the addition of internal solvent standards, solvents with increased sensitivity of detection, online hyphenation of sample preparation, and separation and detection of samples for parallel batch operations. The air monitoring of gaseous samples provide concentration of the analytes on an adsorbent or sorbent, followed by thermal desorption replacing classical adsorption followed by liquid desorption. The miniaturized extraction method using pressurized liquid extraction (PLE) or superheated water extraction, extracts small solvent sample amounts with a limited amount of organic solvent or water.