Optimization of binaphthyl enantiomer separations by capillary zone electrophoresis using mobile phases containing bile salts and organic solvent
✍ Scribed by Cole, Roderic O. ;Sepaniak, Michael J. ;Hinze, W. L.
- Publisher
- John Wiley and Sons
- Year
- 1990
- Tongue
- English
- Weight
- 425 KB
- Volume
- 13
- Category
- Article
- ISSN
- 0935-6304
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✦ Synopsis
It is probable that some contaminants will not respond to the FPD and thereby invalidate any purity calculation. However, this detector is very useful in detecting the presence of any tin compounds in addition to the one of interest during the purification steps. The high sensitivity of HRGC/FPD makes it useful for residues analysis if certain precautions are taken. The peak tailing of alkylated organotin compounds, also observed by other authors [3-41, appears to be related to the internal spatial dimensions and prior use of the FPD [5]. Therefore, the peaks heights of sample and standard should be matched within 25 % to minimize error in quantitation. Figure 8 shows a chromatogram of 7 pentyl-, phenyl-, and cyclohexyl-tin compounds at approx. 200 pg each (28-30 pg Sn).
Percent purity values, calculated on the ion trap detector in the electron impact total ion mode, are shown in Table 2 with the major contaminants identified and quantified.
4 Conclusions
A method has been described for the preparation, purification, and characterization of the pentyl derivatives of the phenyl-and cyclohexyl-tin chlorides. Fortunately, HPLC fractionation of the di-and tri-cyclohexylpentyl tins was not necessary since these do not respond to UV detection. Pentyl-rather than phenyl-derivatization was chosen so that triphenyltin hydroxide and triphenyltin acetate residues could be differentiated from tetra-phenyltin residues, which have been reported as present in the environment.