Silver compounds mass spectra

Fig. 8.19. Coordination ion spray mass spectrum of estradiol extracted from the reversed-phase CEC—CIS-MS separation of estrogenic compounds. Column, 250 x 0.1 mm i.d. packed with 3 pm GROM-SIL ODS-O AB eluent, 4 mmol/1 ammonium acetate, pH 9.0, 50% acetonitrile applied pressure, 8 MPa applied voltage, 15 kV detection, ESI-MS, 0.85 s/spectrum sheath liquid, 100 pg/ml aqueous silver nitrate, 3 pl/min mass spectrum extracted from a reconstructed ion chromatogram of the separation of estriol, estradiol, equiline, and estrone. (Reproduced from ref. [104] with permission of Wiley-VCh).

Figure 2 shows the chromatogram of the starting reaction product, Ce C82(CF3)x. Three Ce C82(CF3)5 isomers were isolated from fractions A, B, D and pure Ce2 Cgo was isolated from fraction D. In contrast to the reaction of Y-EMFs with silver (I) trifluoroacetate, which affords two Y C82(CF3)5 isomers and Y2 Cg0(CF3)13 derivatives [12], the reaction with Ce-EMFv affords three Ce Cg2(CF3)5 isomers and Ce2 Cg0 does not react and can be isolated as an individual compound. The F1PLC chromatogram and the Sg-MALDI spectrum of isolated Ce Cg2(CF3)5 (isomer III) are presented in Fig. 3. The mass spectrum shows only the peak with m/z=1469 attributable to Ce Cg2(CF3)5+. The fragmentation of this ion results in the loss of the CF3 groups up to the formation of the Ce C82+ ion. The 99 % purity of Ce C82(CF3)5 (isomers I, II and III) and Y Cg2(CF3)5 (isomers I and II) was determined by HPLC and Sg-MALDI analysis.

Despite its low volatility, silver trifluoromethanesulfonate (38) gave an El mass spectrum with intense [M + Ag] + ions, leading to the suggestion that 38 vaporized as a dimer34. FD mass spectra of both 38 and silver methanesulfonate (39) showed the presence of cluster ions [nM + Ag]+, with n = 1-6 for 38 and n = 1-7 for 3935a. Each cluster ion yielded multiple peaks with relative intensities determined by the presence of the silver isotopes. A mixture of the two compounds showed a FD mass spectrum comprising additional clusters with mixed anions. Thus, the resulting spectrum had relatively intense... 

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