RE: Internal standard

Leigh, Scott (uunet!cson.com!SLeigh@mail.uu.net)
Mon, 17 May 1999 10:32:20 -0700

Debora - You could make a phenylthiocarbamyl derivative of any amino acid,
as in the Pico-Tag method of amino acid analysis. This would give a wide
choice of potential internal standards with different retention times, some
of which might work well with your organic modifier and mobile phase.
Basically you just react Phenylisothiocyanate (PITC) with any one amino acid
to get the phenylthiocarbamyl (PTC) derivative. The PTC derivatives have a
maximal absorbance at 254 nm. The only question in my mind would be how
stable these derivatives are over time. You could probably store the PTC-AA
at -20oC in aliquots for long periods of time. There are a number of
references out there on doing the chemistry - a good reference would be
Bidlingmeyer, Cohen, and Tarvin, J Chromatogr 336, 93-104, 1984.

Scott Leigh, PhD
Cohesion Technologies
2500 Faber Place
Palo Alto, CA 94303
Phone (650) 354-4847
Fax (650) 856-0533
sleigh@cson.com

> -----Original Message-----
> From: Debora Fontanini [SMTP:dfontani@facstaff.wisc.edu]
> Sent: Saturday, May 15, 1999 8:00 PM
> To: Recipients of ABRF List
> Subject: Internal standard
>
> Dear ABRFs,
>
> I am not sure this is the best place to post my question, but many of you
> seem very familiar with HPLC techniques, adn I hope somebody can help me;
> here is my question:
> I am analyzing the activity of an enzyme in the process of being purified,
> using an HPLC assays; the reaction products are analyzed by separation on
> a
> Zorbax C-18 column, using the following gradient: 0.1% TFA (A) in water
> with 20% of 0.1% TFA (B) in acetonitrile, going up to 50% in 14 minutes.
> The substrate and the products elutes at about 35% of B.
> To accurately quantify the amount of digestion, in presence and without a
> particular inhibitor, I need to use an internal standard. I have tried
> various compounds, included benzene which would work out just fine if it
> was not so volatile that by the time is injected (after a 2 hrs reaction),
> is all gone.
> Can any of you think of something that I could use in my reaction and
> inject as a standard, which possibly elutes before my substrate (I would
> like not to use a longer gradient, if avoidable) and absorbs nicely at
> 254nm?
>
> Any help is greatly appreciated,
>
>
> Debora Fontanini-Sella
> University of Wisconsin-Madison
> e-mail: dfontani@facstaff.wisc.edu
> phone: (608) 262-4478