Author Topic: Different Tests for Presence of Alkaloids.  (Read 158 times)

LYC

  • Pupae
  • **
  • Posts: 55
Different Tests for Presence of Alkaloids.
« on: June 11, 2010, 09:03:05 PM »
I didn't want to hi-jack anyone's threads, but this relates to the thread about the van urk solution, as well as possibly being useful/related to the ergot thread if there were ever an interest in trying to find a strain of it with high alkaloid productions.

I'd like to see as many different tests for alkaloids, and summaries such as the van urks reagant, etc.

First Reference: Useful:

http://webcache.googleusercontent.com/search?q=cache%3Ar-RzhU0f42AJ%3Awww.pua.edu.eg%2FPUASite%2Fuploads%2Ffile%2FPharmacy%2Fspring2010%2FPHR344%2Fweek3%2Fpractical%25203.pdf+Erdmann+alkaloid+test&hl=en&gl=us

From: http://resources.metapress.com/pdf-preview.axd?code=01307k9616111681&size=largest

    *  Classification of Alkaloidal precipitating agents:

1- Reagents that form double salts:

    a- Mayer’s Reagent: Potassium Mercuric Iodide.

    b- Dragendorff’s Reagents: Potassium Iodobismethate.

    c- Gold Chloride.

2- Reagents Containing Halogens:

    a- Wagner’s Reagent: Iodine/ Potassium Iodide.

3-Organic Acids:

    a- Hager’s Reagent: Picric Acid

    b- Tannic Acid.

4- Oxygenated High Molecular Weight Acids:

    a- Phosphomolybdic acid

    b- Phosphotungestic acid

    c- Silicotungestic Acid
 
 
 
 

    * Colour Reagents:

 

      1- Froehd’s Reagent: Phosphomolybdic acid

      2- Marqui’s Reagent: Formaldehyde/ Conc. H2SO4

      3- Mandalin’s Reagent: Sulphovanidic acid

      4- Erdmann’s Reagent: Conc. HNO3/Conc. H2SO4

      5- Mecke's Reagent: Selenious acid / conc. H2SO4

      6- Shaer's Reagent: Hydrogen peroxide / conc. H2SO4

      7- Rosenthaler's Reagent: Potassium arsenate / conc. H2SO4

      8- Conc. HNO3

Another useful link with other tests... http://resources.metapress.com/pdf-preview.axd?code=01307k9616111681&size=largest

I/we will need to add how to make, use and expect for these reagents.

This could also come in very useful when it came to finding a magic mushroom that contained higher alkaloids then general via the testing the mycelium of various strains.

Naf1

  • Foundress Queen
  • *****
  • Posts: 753
Re: Different Tests for Presence of Alkaloids.
« Reply #1 on: June 11, 2010, 11:00:35 PM »
Process for the presumptive identification of narcotics and drugs of abuse
United States Patent 4104027

A process is provided for the presumptive identification of narcotics and drugs of abuse, utilizing a combination of color-producing reagents in a sequence which minimizes the occurrence of false positives, and makes possible the presumptive identification by color matching of virtually all the important narcotics and drugs of abuse found in traffic at the present time.



http://www.freepatentsonline.com/4104027.html
http://www.freepatentsonline.com/4104027.pdf

LYC

  • Pupae
  • **
  • Posts: 55
Re: Different Tests for Presence of Alkaloids.
« Reply #2 on: June 11, 2010, 11:28:40 PM »
great links and info! thank you. :)

Are there any reagents, or methods to not only detect the presents of alkaloids, but to do so in a semi-quantitative way? such as item X has more alkaloids present then item Y
No idea how that could work, but I guess only by intensity of color from the test... It seems like the alkaloid present in the reaction would need to be the limiting factor of course. I don't know.

Naf1

  • Foundress Queen
  • *****
  • Posts: 753
Re: Different Tests for Presence of Alkaloids.
« Reply #3 on: June 11, 2010, 11:43:09 PM »
Well TLC gives a decent idea to the proportions, once you develop the plate by spraying on a suitable color reagent. For example take the cannalytics fingerprint kit,

Above is an example of a TLC plate that has been sprayed with Fast Blue B Salt, the Rf values have been replaced with the name of the compound. So is easier to use, they then supply you with a small chart that is used to determine (roughly) what % THC the sample is by the relative size of the dot. They took samples of known % and used that method and recorded the size of the dot a sample of known size and potency produced.

Although this guy was a horrible photographer, you can see that different samples produced different sized dots (relating directly to THC content of the sample).

http://www.icmag.com/ic/showthread.php?p=3133319

« Last Edit: June 11, 2010, 11:49:54 PM by Naf1 »

Quantum Dude

  • Subordinate Wasp
  • ***
  • Posts: 192
Re: Different Tests for Presence of Alkaloids.
« Reply #4 on: June 11, 2010, 11:52:42 PM »
Couldnt help but notice that the chen's test was missing or maybe I read too fast. Enables one to discriminate between amphetamine & methamphetamine versus ephedrine, pseudoephedrine and phenylpropanolamine. The latter 3 gives a purple color wheras amphetamine and methamphetamine give no results.


Reagent Name: Chen's Test

REAGENT PREPARATION

Reagent 1: Add 1 ml of glacial acetic acid to 100 ml of water (=1% (v/v) aqueous acetic acid solution).

Reagent 2: Dissolve 1 g of copper (II) sulphate in 100 ml of water (=1% (w/v) aqueous CuSO4 solution).

Reagent 3: Dissolve 8 g of sodium hydroxide in 100 ml of water (=2N aqueous sodium hydroxide solution).

PROCEDURE

- Place a small amount (1-2 mg of powder, or 1-2 drops of a liquid) of the suspected material in a depression on a spot plate.

- Add 2 drops of Reagent 1.

- Add 2 drops of Reagent 2, then add 2 drops of Reagent 3 and stir.

- Observe the color of the mixture.

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Different Tests for Presence of Alkaloids.
« Reply #5 on: June 12, 2010, 12:04:52 AM »
Is the color change quantative? IE will a little purple VS aldarkpurple allow one to estimate the completion of a reaction. Is there any knowledge of this being used in developing a TLC plate where it would come in handy greatly.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Quantum Dude

  • Subordinate Wasp
  • ***
  • Posts: 192
Re: Different Tests for Presence of Alkaloids.
« Reply #6 on: June 12, 2010, 12:10:43 AM »
Is the color change quantative? IE will a little purple VS aldarkpurple allow one to estimate the completion of a reaction. Is there any knowledge of this being used in developing a TLC plate where it would come in handy greatly.
thats some good thinking but I highly doubt so....purely qualitative.

AMPHETAMINE, METHAMPHETAMINEAND THEIR RING-SUBSTITUTED
ANALOGUES IN SEIZED MATERIALS, MANUAL FOR USE BY NATIONAL DRUG TESTING LABORATORIES

Naf1

  • Foundress Queen
  • *****
  • Posts: 753
Re: Different Tests for Presence of Alkaloids.
« Reply #7 on: June 12, 2010, 12:18:13 AM »
You could just run a TLC plate at the start where obviously one big purple pseudo dot will be visible, and as the reaction runs you could monitor it by taking tiny samples with a capillary tube. The big dot would get smaller as the reaction carries on, if you did two small plates at the same time and just used different visualization agents spraying one with easily available Dance safe kit (marquis or mecke ect)would be fine for the second (you can cut TLC plates into thin strips, spray one with Chens and one with Marquis). BTW; If the color reaction works, it can be sprayed onto TLC plates to visualize! Filter paper is an excellent substitute for TLC plates.

[youtube]http://www.youtube.com/watch?v=DxfygUL8k3Y[/youtube]
« Last Edit: June 12, 2010, 12:28:23 AM by Naf1 »

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Different Tests for Presence of Alkaloids.
« Reply #8 on: June 14, 2010, 07:07:31 PM »
There is also the Salkowski reaction.

Quote
After the reverse side is sprayed with a reagent
consisting of 1 ml of 1.5 M FeCl3 solution and 100 ml of
60%o sulfuric acid, the colony is incubated at 60°C for 5
min. The intensity of the blue color which develops
corresponds to the amount of alkaloid present.

This looks easy to make, and useful -- I don't know if it works for all alkaloids, probably not, but it does for ergot alkaloids.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Tsathoggua

  • Autistic sociopath
  • Foundress Queen
  • *****
  • Posts: 662
Re: Different Tests for Presence of Alkaloids.
« Reply #9 on: June 14, 2010, 09:47:16 PM »
I think I might try this on some mashed up sclerotia, just a couple to try and observe the reaction in process.

Another suggested reagent test to include is the meixner test for amatoxins, the deadly cyclic peptides from Amanita phalloides, A.ocreata, A.virosa, A.bisporigera etc.

Concentrated HCl dropped into a patch of blotting paper that has had a piece of the fungus mashed onto it, the paper must be high in lignin, some newspaper is suitable for use also, after some time, a blueish ring will develop around the fungal tissue if amatoxin is present.

interestingly, I heard an anecdote that it isn't suitable for telling suspicious psilocybin fungi from amatoxin bearing species such as Galerinas, Conocybe filaris as it may cross react.

Can anybody attest to this? I don't happen to keep deadly amatoxic fungi around in my fridge, sorry, I need all the room for my ergot samples.
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

LYC

  • Pupae
  • **
  • Posts: 55
Re: Different Tests for Presence of Alkaloids.
« Reply #10 on: June 15, 2010, 04:37:30 AM »
Isn't amatoxic fungi fairly common in lawns and such? Might get lucky and be closer to it then you think.

Tsathoggua

  • Autistic sociopath
  • Foundress Queen
  • *****
  • Posts: 662
Re: Different Tests for Presence of Alkaloids.
« Reply #11 on: June 17, 2010, 09:44:10 PM »
Hmmm...Lepiota species! fuck why didn't I think of that.

There are a fair few species that grow here, L.cristata is fairly common in some nearby woods.
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

Naf1

  • Foundress Queen
  • *****
  • Posts: 753
Re: Different Tests for Presence of Alkaloids.
« Reply #12 on: June 18, 2010, 12:19:13 AM »
A gift from 'The Home Scientist'

Testing for Alkaloids with Dragendorff Reagent, the home scientist demonstrates how to use Dragendorffs reagent for testing for the presence of alkaloids.
[youtube]http://www.youtube.com/watch?v=RwVWpGPiu9k[/youtube]
Hint;Keep an eye out for the alternate recipe, replacing the expensive bismuth nitrate with pepto bismol.
« Last Edit: June 18, 2010, 06:00:43 AM by Naf1 »

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Different Tests for Presence of Alkaloids.
« Reply #13 on: July 02, 2010, 10:39:16 PM »
Quote
Hint;Keep an eye out for the alternate recipe, replacing the expensive bismuth nitrate with pepto bismol.
Copied from the youtube page for the sake of convenience and preservation.

Quote
1. Transfer two Pepto-Bismol tablets and about 20 mL of water to a beaker.

2. Swirl the beaker until the tablets have broken up into powder. Bismuth subsalicylate and the binders used in the tablets are both very insoluble in water, so don't be concerned if it looks as though none of the powder has dissolved.

3. Add about 10 mL of concentrated hydrochloric acid to the beaker. Swirl the beaker occasionally until foaming ceases. At this point, the liquid appears chalky white.

4. Allow the contents of the beaker to settle. Most of the solid matter precipitates, but enough remains suspended to give the liquid a cloudy white appearance.

5. Filter or carefully decant the liquid into a second beaker to remove as much as possible of the undissolved solids.

6. Dissolve about 7.0 g of potassium iodide in a few mL of water and transfer that solution to the beaker that contains the bismuth solution. The solution immediately assumes a yellow-brown, cloudy appearance.

7. Bring up the volume in the beaker to about 100 mL with distilled water, allow the solid material to settle, and then pour off the clear yellow-brown solution into a storage bottle labeled Dragendorff Reagent.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

POSEIDON

  • Subordinate Wasp
  • ***
  • Posts: 116
Re: Different Tests for Presence of Alkaloids.
« Reply #14 on: July 14, 2010, 04:26:14 AM »
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim