lets see...just some off the top of my head:
The Mothers Of Invention - Mothermania: The Best of the Mothers (only released on vinyl in 1969)
The Mothers Of Invention - The **** Of The Mothers (1 of 3 official un-official Mothers vinyl compilations released by Verve records without Zappa's consent)
FZ - 12" picture disc single for You Are What You Is, it was shoved in along another Zappa record i bought?!
Gut - Hyper-Intestinal Vulva Desecration, 2nd press on clear green vinyl, the most i ever payed for one 7"
Butthole Surfers - s/t and Live PCPPEP, respectively
Grateful Dead - Historic Dead
Nazarene Whore - Ritual of Anus cassette, #2/30 hand numbered
as for cds, off the top of my head:
both Pathologist albums
Gore - Consumed by Slow Decay
Captain Beefheart - Live 'n Rare hand numbered
Cattle Decapitation/Armatron/Ticwar split, seemingly impossible to find
there are more i'm sure, i have a lot of music in storage and its early so i cant think 100%