Ammonium Hydroxide → Gossypol
反応式
[NH4+].[OH-:2].[CH3:3][C:4]1[CH:9]=[C:8]2[C:10]([CH:24]([CH3:26])[CH3:25])=[C:11]([OH:23])[C:12](/[C:14](=[CH:15]\NC3C=CC=CC=3)/[C:7]2=[C:6]([OH:27])[C:5]=1[C:28]1[C:33]([OH:34])=[C:32]2[C:35]([CH:44]=[O:45])=[C:36]([OH:43])[C:37]([OH:42])=[C:38]([CH:39]([CH3:41])[CH3:40])[C:31]2=[CH:30][C:29]=1[CH3:46])=[O:13]>CO>[CH3:3][C:4]1[C:5]([C:28]2[C:29]([CH3:46])=[CH:30][C:31]3[C:38]([CH:39]([CH3:41])[CH3:40])=[C:37]([OH:42])[C:36]([OH:43])=[C:35]([CH:44]=[O:45])[C:32]=3[C:33]=2[OH:34])=[C:6]([OH:27])[C:7]2=[C:14]([CH:15]=[O:2])[C:12]([OH:13])=[C:11]([OH:23])[C:10]([CH:24]([CH3:26])[CH3:25])=[C:8]2[CH:9]=1参加物
4
実験手順
The mass spectrometer was a Micromass Quattro Ultima LC/MS/MS detector by Waters, and contained a triple quadrupole mass spectrometer with negative electrospray ionization. Because the HPLC did not provide the correct ionization matrix for negative electrospray ionization of the dianilino-gossypol, 0.6% NH4OH in methanol was introduced past the HPLC column at a flow rate of 0.05 mL/minute. Post-column mixing of the NH4OH in MeOH with the HPLC eluant was achieved using a mixing T-connection. In MS/MS mode, the first quadrupole was used to select 667.3 as the mass to charge ratio that represented the negative ion of dianilino-gossypol. In the second quadrupole, the 667.3 mass to charge ratio was fragmented in a collision cell. The third quadrupole was used to select the fragment ion, monoanilino-gossypol, which had a mass to charge ratio of 574.2 as a result of the loss of an aniline. Detection of the second fragment ion provides improved specificity and increased signal to noise ratios.