Re: Digest/ProtSeq

Gautam Sarath (gsarath@unlinfo.unl.edu)
Mon, 2 Mar 1998 13:57:42 -0600 (CST)

Rebecca: I have encountered a lot of problems with heavily
glycosylated proteins, also with 1 lightly glycosylated protein, based
on these experiences, I always have a positive control (e.g.,
myoglobin) during all tryptic digests, if nothing else, I know the
enzyme worked. The other possibility is that you indeed have too
little sample. If the need is to obtain some kind of confirmatory
sequence data, why not put the digest onto a LC/MS?. Alternatively,
you could perform a limited-time digest with a broad specificity
endopeptidase such as thermolysin etc and separate released peptides.
In my hands, low levels of protein have not been good sources for CNBr
digestion, although one possibility is to try the gas phase CNBr
cleavage of PVDF-immobilized protein, and elute digested proteins into
1% TFA/80% acteonitrile and separating these by microcapillary HPLC. I
do not have one of these beasties and so my limitation has been the
narrowbore/microbore C-18 column and an old detector. Hope this helps,
and I know several other good <underline>suggestions are on the way,
gautam sarath </underline>

>A customer brought me a Coo-blue stained blot with a faint but visible
band on

>it to sequence. I put it on my sequncer and got no sequence. I told
the

>customer that either there was less protein in the band than we
thought or it

>was N-terminally blocked.

>

>We sequenced again with (she tells me) more sample -- still no
sequence. We

>decided that it must be blocked and decided to digest it.

>

>The expected protein has plenty of tryptic sites so we red/alk and
then did a

>tryptic digest(on PVDF). (DTT/Iodoacetate, Promega trypsin) I ran
the digest

>on a sample slice and a blank slice (of PVDF) in parallel. When I ran
the

>digests out on my microcapillary HPLC, the digest of the sample PVDF
looked

>exactly the same as the digest of the blank lane. I have to conclude
that the

>protein didn't digest, but why ?

>

>At this point my customer only has a little bit of the sample left (we
only

>get 1 more shot). She needs enough sequence to prove that the protein
is what

>her western's have led her to believe it is.

>

>My questions:

>

>1) Are there proteins out there that are Trypsin resistant even
after

>reduction/alkylation ?

>

>2) What other possible explanations are there ?

>

>3) What would you do next ? (Our only idea is to try CNBr?)

>

>Thank you all for all the past help and thanks in advance for help
with this

>problem.

>

>Weather Inconsequential(Charleston S.C.):

>Spring has sprung and if you can avoid sinking up to your ankles in
mud, the

>azaelas are beautiful !

>

>Rebecca P. Ettling

>Biotechnology Resource Laboratory

>Protein Sequencing and Peptide Synthesis Facility

>Department of Biochemistry (Rm 505)

>Medical University of South Carolina

>171 Ashley Avenue,

>Charleston, SC 29403

>Tel.: (803) 792-1271

>Fax: (803) 792-1264

Gautam Sarath

N-226, Beadle center

Protein Core Facility

Department of Biochemistry

University of Nebraska-Lincoln

Lincoln, NE 68588-0664

Phone: 402-472-2928

FAX: 402-472-7842