CHATPRIVACYDONATELOGINREGISTER
DMT-Nexus
FAQWIKIHEALTH & SAFETYARTATTITUDEACTIVE TOPICS
HPLC analysis of psilocin/psilocybin Options
 
benzyme
#1 Posted : 6/7/2018 4:25:49 AM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
http://booksc.org/book/4147048/b92bbe

This procedure was replicated by sonication @ 80W, of a dry gram of p.cubensis aborts in ~50 mL hplc-grade methanol for 10 mins at 25 C , followed by magnetic stirring for 24 hr. The solution was filtered through 0.44 um syringe filters into 1.5 mL autosampler vials. HPLC-UV analysis was conducted isocratically, the mobile phase consisted of 10:90:1 MeOH:H2O:AcOH, at 333 uL/min. @ 25C. Excitation wavelength was 283 nm. The column used was a Phenomenex Kinetex C18 100x2.1mm, 2.6um 100Å.

The implications are clear. This is a potency/purity assay that would be very useful for biotransformation studies.

The bottom chromatogram is an ongoing investigation, as six fractions were collected for further analysis. Separation was done with a ramp gradient from 100% of the aforementioned mobile phase, to 100% of 0.1% Formic acid in Acetonitrile, over the course of 10 mins, holding at the latter mobile phase for the duration.
benzyme attached the following image(s):
IMG_4830.jpg (2,767kb) downloaded 264 time(s).
IMG_4840.jpg (2,312kb) downloaded 225 time(s).
IMG_4848.jpg (3,222kb) downloaded 220 time(s).
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
benzyme
#2 Posted : 7/27/2018 5:13:51 AM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
The same mobile phase was used, at 0.3 mL/min. The samples, 0.5g of controls and 0.5g experimental (10mM tryptamine hcl) aborts, were homogenized in 10mL hplc-grade methanol, and centrifuged @ 5000rpm for 5 min. Aliquots of 100uL from each were diluted with 900uL MeOH; 10uL injections were analyzed, 286nm excitation.

the first three are controls, the second three are experimental; notated in area counts. Taking the mean of the counts, the experimental group resulted in 6% increase in psilocybin.
benzyme attached the following image(s):
IMG_5143.JPG (329kb) downloaded 205 time(s).
IMG_5145.JPG (113kb) downloaded 204 time(s).
IMG_5147.JPG (145kb) downloaded 205 time(s).
IMG_5144.JPG (590kb) downloaded 204 time(s).
IMG_5146.JPG (142kb) downloaded 202 time(s).
IMG_5148.JPG (154kb) downloaded 203 time(s).
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
benzyme
#3 Posted : 7/28/2018 11:28:18 PM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
today 1.5mL aliquots from the stock sol'n were taken, and the result was a 9.125% difference between the respective area counts.

there appears to be a direct correlation to the addition of dopant, and the augmentation of area counts. Further experiments will be conducted with 15mM tryptamine hcl.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Nitegazer
#4 Posted : 9/14/2018 3:02:59 PM

DMT-Nexus member


Posts: 368
Joined: 09-Jun-2011
Last visit: 27-Nov-2020
Benzyme--

You are in waters way beyond my depth, but I may have bumped into a paper that would be germane to your work. "Determination of Psilocybin and Psilocin in Hallucinogenic Mushrooms by HPLC with Diode Array and MS Detection"(2008 )

Here is a link to the article, and I'll try to attach it below.

https://www.thevespiary.org/rhod...and-MS-Detection1b3b.pdf

I've been trying to untangle the myths around the lemon tek, and am amazed at how little is known about the quantities of psilocin and psilocybin in the mushroom or dephosphorylation of psilocybin to psilocin.

Hope this is at least a bit helpful. I greatly appreciate your work.
 
benzyme
#5 Posted : 9/14/2018 3:16:17 PM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
thank you, sir. Big grin
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
benzyme
#6 Posted : 9/17/2018 2:04:50 PM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
after doing some reading, I discovered that the small peak that co-elutes with the large peak is baeocystin.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Myco
#7 Posted : 9/21/2018 8:10:01 PM

73μ


Posts: 103
Joined: 04-Dec-2010
Last visit: 03-Aug-2019
Location: Hyperion
Thank-you for your work Benzyme.
arrive without traveling.
 
benzyme
#8 Posted : 9/21/2018 11:53:28 PM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
You're most welcome. It's what I do when I'm not 'at work'.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Loveall
#9 Posted : 9/29/2018 9:36:24 PM

💖

Chemical expertSenior Member

Posts: 2450
Joined: 11-Mar-2017
Last visit: 27-Oct-2021
Location: 🌎
What about psiclocin content? Gartz found a huge boost to psiclocin content when he doped with 25mM of tryptamine HCl.

I love this work by the way. Thank you for doing it benzyme.
 
benzyme
#10 Posted : 9/30/2018 12:27:42 AM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

Posts: 7295
Joined: 21-May-2008
Last visit: 27-Oct-2021
Location: the lab
I didn't do the math, but the second peak is psilocin, and there is an increase in counts. It's only 10mM supplementation.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Loveall
#11 Posted : 9/30/2018 7:30:59 PM

💖

Chemical expertSenior Member

Posts: 2450
Joined: 11-Mar-2017
Last visit: 27-Oct-2021
Location: 🌎
Right, it's just interesting that at 25mM a very large psiclocin increase was seen back in 1989.
 
 
Users browsing this forum
Guest

DMT-Nexus theme created by The Traveler
This page was generated in 0.025 seconds.