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Author Topic: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)  (Read 1616 times)

Vesp

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #160 on: May 08, 2011, 07:05:47 PM »
Something went wrong with this thread and so I deleted and modified a few posts - I don't think anything was important - just double posts and questions asking about this thread being broken... fixed now though...
« Last Edit: May 08, 2011, 07:07:31 PM by Vesp »
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aniracetam

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #161 on: May 09, 2011, 05:57:08 PM »
the metabolic pathway was actually relevant, as i continue to post spectral data.
 it's an indicator of which byproducts are likely being separated.

in any event, I ran ESI-MS on an extraction from a new batch (4 days old), and got a strong signal for 353 m/z.
odd, because the only ergoline i can find with that mass is methysergide...

(oh crap.. just realized..the amber bottle I put the sample in had residual diethylamine, though I rinsed it with IPA. the sample was basified with conc. NH4OH in MeOH, extracted with xylene, then extracted with tartaric acid in MeOH and transferred to that bottle)


yea, I know..the background is fairly noisy, but the signal-to-noise ratio is two orders of magnitude.
the background base peak is 474.4, sample base peak is 353.2.
« Last Edit: May 09, 2011, 06:35:14 PM by aniracetam »
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overunity33

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #162 on: May 21, 2011, 06:38:28 AM »

whos gona make this thing for the seed culture?

ender

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #163 on: May 22, 2011, 05:00:40 AM »
Quote from: aniracetam on May 08, 2011, 03:41:13 AM
I hear ya

I'm gonna have to finagle one. been working with them for about two years, and know what to look for in one.
was able to differentiate between THH and harmine (seen in the attachment) in a sample using an LCQ, which I've seen go for 2800 - 7500 on 3bay.
already bought a harvard apparatus 22 series LC syringe pump for $130

You can pick up a cheap dispersive IR instrument that does a decent job of ID'ing samples such as harmine.  The one that run these spectra of harmaline and DXM cost about $100.  The resolution exceeds my reference library spectra.





- ender
« Last Edit: May 22, 2011, 05:23:44 AM by ender »

overunity33

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #164 on: May 22, 2011, 07:17:18 AM »
Where do you find one of these 100$ units?  Since its the same type of setup as UV-vis could you get one with a detector/grating that could be easily switchable between the two?  havent done too much reading on it but it sounds worthwhile. id love to hear more.

ender

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #165 on: May 22, 2011, 08:34:42 AM »
No, the source and detector are different between the two instruments.  That specific IR instrument is described in the following website:

hxxp://antiquesci.50webs.com/PE337/PE337-1.htm

Instruments of that type come up on auction occasionally.  Since they're quite heavy, you have to get lucky and have one show up AND have it close enough to go pick it up in person without paying freight charges which can run into the hundreds depending on the distance.  It might take years to get that lucky, but not if you're living in or near a major city with a lot of industry.  Some experience and skill at troubleshooting electronics and mechanisms helps as a lot of stuff is broken that you can get cheap on auction.

You'll also need to capture the detector signal which is a DC voltage using some sort of data acquisition device.  But those can be had cheap.  For example this one, at $29, would be adequate:

hxxp://www.dataq.com/products/startkit/di145.html

Even comes with software.

So there's some thought and perhaps years of patience that goes into it, but the technology is definitely out there.

- ender
« Last Edit: May 22, 2011, 08:47:30 AM by ender »

aniracetam

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #166 on: May 22, 2011, 05:49:20 PM »
hell, I'd love to have an FTIR, but I've never seen them cheaper than $400. I saw a Nicolet Impact 410 with software sell recently for $898, not including shipping.

I'll probably pass on an FTIR, and eventually obtain an LC-MS/MS (from contacts) instead, it's a much more powerful method of characterization. they're definitely not cheap, but I've seen a complete Finnigan LCQ system with a workstation running Excalibur sell for $2700. I love those machines; very easy to maintain, imo

a multifunction DAQ module is a handy alternative for control and acquisition from instruments which don't come with software. It may require some low-level programming, but it works
« Last Edit: June 23, 2011, 04:06:35 AM by aniracetam »
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aniracetam

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #167 on: June 23, 2011, 03:57:28 AM »
here's a microscale chrom separation of tartrate salts treated with Van Urk's. Eluent is EtOAc.
« Last Edit: June 23, 2011, 04:08:17 AM by aniracetam »
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aniracetam

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #168 on: July 06, 2011, 04:26:23 PM »
ergot alks, tartrate salt form in EtOH.

van urk's spot test (control is the light dot in the lower left part of the filter, it's just van urk's reagent)
« Last Edit: July 06, 2011, 04:28:11 PM by aniracetam »
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Vesp

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #169 on: July 06, 2011, 07:44:04 PM »
Very nice - you have now extracted it? How many mg do you think you have obtained?
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aniracetam

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Re: Ergot Culture Medium for Alkaloid Production (C. Purpurea & Paspali)
« Reply #170 on: July 06, 2011, 08:04:31 PM »
2000+  mg
"Experiments are the only means of knowledge at our disposal. The rest is poetry, imagination." - Max Planck
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