HPLC coupled with other spectrometric detectors

3 HPLC coupled with other spectrometric detectors 

Compared with the ICP, other atomic spectrometric detectors are not widely coupled to HPLC. Several interfaces have been described for AAS detector. Methods include a rotating platinum spiral collection system (Ebdon et al., 1987) and a flow injection thermospray sample introduction system (Robinson and Choi, 1987). Post-column hydride generation is also popular with AAS detection as will be described later. Pedersen and Larsen (1997) used an anion-exchange column to separate selenomethionine, selenocysteine, selenite and selenate with both FAAS and ICP-MS. The detection limits for the FAAS system were lmg H1 compared with 1 fig l-1 for ICP-MS. HPLC-MIP systems have been described to an even lesser extent. These either use elaborate interfaces to overcome the problems of quenching the low-power plasma (Zhang and Carnahan, 1989) or use a modified argon/oxygen mixed gas plasma (Kollotzek et al., 1984). 

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In addition to the spectrometric detectors, HPLC has also been coupled with other detection systems, such as mass spectrometry (MS). Specificity can be highly improved using tandem mass spectrometry (HPLC-MS/MS) (Holler et al. 2006 Yomota and Ohnishi 2007). High sensitivity and selectivity can also be achieved by HPLC coupled with electrochemical detection (Kucera et al. 2007). 

GC analyses of the pupal secretion of E. borealis have indicated the presence of vitamin E acetate and other tocopherol derivatives [49,50]. However, in tests with ants, these compounds proved to be essentially inactive, whereas the secretion itself was potently deterrent. To find and identify the active components in the pupal Epilachna borealis secretion, NMR spectroscopic studies on the fresh secretion were carried out. One and two-dimensional NMR experiments revealed that the tocopheryl acetates account for only a relatively small percentage of the beetles5 total secretion (20%), whereas the major components represented a group of previously undetected compounds. By analysis of the COSY, HSQC and HMBC spectra of the mixture, these components were shown to be esters and amides derived from three (co-l)-(2-hydroxyethylamino)alka-noic acids 44-46. HPLC analyses coupled to a mass spectrometric detector revealed that the secretion contain a highly diverse mixture of macrocyclic polyamines, the polyazamacrolides (PAMLs) 47-52 (Fig. 8). 

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