Microchemical separation techniques

Because of the small amounts of sample that are usually obtained, coupled GC-MS is the method of choice for analysis of volatile pheromones. The analysis of the less-volatile lipids and polar pheromone components may require derivatization and microchemical tests, both to improve chromatographic characteristics and to provide information about the structures. It is likely that chromatographic techniques with high separation power and high sensitivity for polar compounds, such as coupled capillary electrophoresis-mass spectrometry, will prove useful for analysis of spider extracts in future studies. 

Chromatographic techniques are the main methods that have been used to separate, detect, and identify organic components of FDR.152 162 Other methods considered include molecular luminescence,163 infrared spectroscopy,164 Raman spectroscopy,165 electron spin response spectrometry,166 microchemical crystal tests,167 168 ultraviolet spectroscopy/nuclear magnetic resonance/polarography.169... 

Although Meinke (603) points out that automation in analytical chemistry is most desirable to remove the drawbacks of radiochemical separations in activation analysis, many other analysts who use activation analysis for trace element determinations in biological materials continue effective research on separation systems for a single element or a small group of elements with similar chemical characteristics for example, the methods and techniques in the publication by Gorsuch (338) have been used by many analysts in their activation analysis determinations of trace elements. Other successful microchemical techniques used in activation analysis have been described by Pijck and Hoste (713), Sion, Hoste, and Gillis (858), Girardi and Merlini (331), and Smales and Mapper (864). 

Integrated microreaction solutions often require fluid pathways on a chip to be altered between different reaction, separation and detection steps. A variety of active valves for fluid control were previously developed in polymers using soft-lithographic techniques [167-169] and, based on metals and silicon, in the MEMS community. Most of these solutions, however, pose significant challenges with respect either to the chemical and thermal compatibility required for many microchemical systems or to fabrication cost and ease of integration. 

The instrumentation became increasingly sophisticated with the addition of provision to heat the column, an automatic titrating device and then the first successful sensitive and universal detector, the gas-density balance, all of which required to be handcrafted [597]. In a companion paper to the description of the detector, the technique was demonstrated with the first separations of methyl ester derivatives of fatty acids [433]. It appears that the initial contact with the problem of the resolution of fatty acids must have inspired James to continue with the study of lipids, and in 1957 he independently published a paper on the determination of the structures of longer-chain fatty acids using gas chromatography and microchemical methods [434]. He subsequently went on to a distinguished career in lipid biochemistry. 

---