Preparative HPLC: Suggested Unit? Like to Collaborate?

[artie mckim]

Hello, everyone. I've been thinking about something, and would like to solicit some some advice.

I'm a synthetic organic chemist, working for a chemical company branching out into some new chemical product lines. My company (Gaylord Chemical Corporation) has a developed competency in GC analysis of our products, but I'm on my own when it comes to HPLC.

I've been successful at rejuvenating an old Waters system for our lab, when the need arose to assay / characterize some new product candidates that are thermally unstable / nonvolatile materials. I'm mechanically inclined, and good at learning new things. So:

I would love to have access to preparative HPLC, but it is hard to rationalize the expenditure at this point in time. I work with another chemist, who runs an academic research group (OK, she's also my girlfriend)- that could also really benefit from preparative HPLC.


If you perform column chromatography on a routine basis, you quickly come to appreciate the promise of preparative HPLC.

[/b]My Questions:

1. Is there a less-than-state-of-the art-model preparative HPLC that someone could suggest, so that I could begin shopping for a used unit? I've had good luck with used / salvaged lab equipment, and having access to a basic preparative HPLC would be wonderful.

It seems like I need suggestions for:

a suitable preparative pump
a UV detector

I can work out the details for the data collection system, and many components would be purchased new (column, tubing, etc.)

2. Is there anyone out there, that has access to a preparative unit, that might be interesting in working with me on various projects? I realize that such work may be contracted out, but it has been my experience that doing so is often quite costly, and that the red tape involved can be frustrating.

In the past, I've had some good experiences collaborating with people that idle instruments, or are finishing up in grad school, or are just interested in doing something new. We can do synthetic work, offer publication co-authorship, or arrange for payment in return.

Cheers!
Artie.

[Mark]

A Waters DeltaPrep 4000 should be available as a used instrument somewhere. I use one with excellent results and the UV is a Waters 486 with a preparative flow cell. These work well, are fairly reliable so far and I would be another one in a heartbeat. You neglected to say what scale you are working at so I just threw this out as a starting point. There are a couple of diferent pump headds available so you can choose your flow range and the unit is advertised for up to 4000 psi (I have used it reliably at 3000 psi without a hitch).

Regards,
Mark

[JM]

If you are only interested in preparative isolation of compounds all you need is a Column, pulse free pump and a UV detector . You can use your existing integrator or chart recorder for ploting. If you are more in to normal phase separation , there are several low end equipments are available in market, but if you intent to use Reverse phase option than you need more than that. For all these types of preparative work , I think schimadzu has one old system LC-8A, which is reliable and not so costly. Though i my self using other preparative systems ( Merck, septech etc) as well, but i feel you need a basic system may be used one.

[Yury Zelechonok]

Since you have Waters system check maximum flow rate on your pump (some analytical Waters models can handle significant flow). If it is 20 mL /min then you can use this pump with up to 1 inch id column. It will be enough for most semi-prep applications. If it just 10 ml/min you still can use 1 inch column working at reduce flow rate conditions which slow you separation two times, but that’s about it in term of negative effect on separation.
You don’t need to do anything with your detector if it is not some sort micro-cell detector. Your autosampler should have a big loop and capacity to inject at least 1 ml sample. You can bypass autosampler with manual injector from Rheodine (cost new $500-700) find one with big channels and grooves.