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Miniaturized sample preparation techniques have been increasingly studied in the research field of separation science due to the possibility to meet the recent requirements such as enhanced sensitivity and selectivity, and more economical and ecological features.The effective hyphenation of the miniaturized sample preparation to microscale separation methods was also investigated, allowing the successful on-line coupling of these techniques without disadvantages typically found in an off-line multistep process for the analysis of complex sample mixtures.For the analysis with gas chromatography (GC), liquid chromatography (LC) and capillary electrophoresis (CE), various types of novel sample preparation techniques have been reported, where most of the works were mainly focused on the increased sensitivity and selectivity of the target compounds with a specially-designed concentration process.Downsizing the sample preparation it makes possible to offer the enhanced mass sensitivity with the reduced sample size, although the suitable optimization of the hyphenated system should be considered.