N&PD Moderators: Skorpio
Can anyone interpret gc/ms results??
egor
Bluelighter
Attached are gc/ms results from spice and chill smoking blends. Unfortunately noone Has access to the library of results with which to compare these as to which compound is the main active constituent. The can d results are from cannabis for the sake of comparasin.
http://www.drugtheory.com/images/spice.pdf
Can anyone tell me what this all means??????
kidamnesiac
Bluelighter
so, maybe im confused here...but it says alk acid base extraction, and he's showing results from cannabis? thc would not be extracted this way, if you have access to a gc/ms and don't know this...but somehow there is a peak @ 314, where THC should be...
it would be nearly impossible for most of us to help you with this data without at least some other characterizations or a list of what is in the spice to begin with. but, for certain, thc is not the major consitunent in the first two. an acid base wouldn't show this anyway, unless you're tossing away the alkaloids...?
good luck
egor
Bluelighter
I had the same question about the cannabis results, it may just be a miss-print. I did not do the test personally, someone I talk to on another forum did it
![:\](https://bluelight.org/xf/BL_Images/Orig_Emoji/wrygrin.gif "wry grin :\")
Without having any knowledge of the compounds involved a GC/MS spectra on it's own is pretty much worthless except when it comes to very simple samples. Real world chemistry isn't exactly as CSI where you can put anything in a machine and get exactly what it's made up of in a matter of seconds. The spectra linked would most definitely need a genius to solve, or more realistically a computer hooked with some good software and databases.
if the GC conditions were the same then it appears to show that chill and spice contain the same ingredient and it is not THC. nor is it HU210 as has been postulated. wthether the major peak seen at 9 minutes something is the active ingredient is uncertain.
this has been done with an ion trap MS so the mass spectra may not be the same as quad mass spec obtained library spectra.
PM me I have a couple of questions.
V
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retired_chemist
Bluelighter
I did GC/MS for an environmental lab for about 5 years. The large number of "grassy" closely spaced ions is characteristic of hydrocarbons. The loss of 30 between the 166+ ion and the 136+ ion suggests decomposition with the extrusion of formaldehyde (MW = 30).
There are no other really useful interperative patterns in the spectra, so my best guess would be some sort of oxygen substituted hydrocarbon.
There are many problems with this analysis:
First problem: A BNA extraction usually involves aqueous extraction under acidic conditions followed by extraction under basic conditions. The combined solvent fractions are N2 vapped down to a concentrate which is then analyzed.
But you have no way of knowing if the "active alkaloid" was even effectively extracted by this process.
Second Problem: Assuming the "active alkaloid" was extracted, did it even elute under the chromatographic conditions? You said it was GC/MS, but there is no information that indicates column type, chromatographic conditions etc. Assuming it was GC/MS all I can say is that many, many organic compounds cannot be analyzed by GC because they are not thermallyt stable enough, cannot be eluted etc.
Just because you see a major peak in the chromatogram does not mean it is even a peak of real interest. For all you know the "active alkaloid" decomposed in the injection port.
Finally I have no clue what Spice or Chill even are, I am assuming some kind of "marijuana" look alike. Assuming this was an extract of a plant material, to be perfectly honest given the major peak appears to be of fairly low MW (no guarantee you are even seeing the parent ion at 166 but there is little spectral information above that) and extrudes formaldehyde, this could be almost anything, plants materials contain all kkinds of low molecualr weight hydrocarbon based aldehydes, alcohols, etc.
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kidamnesiac
Bluelighter
I'm not familiar with spice really, but I know it's smoked, so the compound should be thermally stable enough to make it to the ion detector. Of course, it could decarboxylate or go through a number of other changes before it makes it to your brain or the ion detector.
The point about the major peak not being the major psychoactive portion should be well heeded.
MattPsy
Bluelighter
It won't be HU210 anyway, 'cause as I understand it, HU210 is a full agonist at CB1 and thus should have a very high potential for effect (if enough is taken).
I've tried Spice a few times, experimenting with just how altered you can get with it. You can't get as stoned as cannabis can get you, no matter how much of it you have, suggesting some sort of cut-off level, like what you'd expect from a partial agonist, no?
MattPsy said:
I have a few ideas as to the spice active ingredient(s).
It could indeed be a partial or low affinity agonist. if it is low affinity it may explain oddity number 2.
1)It is a shame that the above GC-MS wasn't a straight quick n dirty non-polar extract, and that there is a chunk of analytical conditions/ experimental information missing.
2) It also strikes me as kind of odd that the one peak is pretty massive under the extraction/ GC-MS conditions, so either spice doesn't contain much else that is extracted under the conditions used or that the 9 minute peak is present in the original sample in massively greater concentrations than the other (plant derived) peaks.
3) The cannabis trace doesn't contain the terpines or other cannabinoids, so I am guessing that the AB extraction is not pulling terpenes or other highly non polar material into the sample, except when the material is in great excess as THC would be in half decent cannabis.
odd odd and thrice odd.
4) and my last observation is that this was most likely done on a student access University machine 
or do these finnigan ion trap machines always have a very high baseline?
Mr Prufrock will no doubt be able to shed light on things, I eagerly await the appearance of that skilled analytic cat
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retired_chemist
Bluelighter
Does not look like they were scanning below 50 so baseline is probably not from an air leak i.e. CO2. Probably a worn out column bleeding liquid phase. This makes the analysis even more suspect, because columns develop active silica sites which can not only adsorb components but can cause a myriad of decomposition reactions.
My impression is that many people not trained in GC/MS actual use suffer from the misunderstanding that it is somehow the end all of analytical techniques. It's not, it is just one of many tools.
A little trick we use to perform to troubleshoot GC problems is instructive in illustrating just how variable GC/MS analysis can be. Now you may think, if you inject a pure sample of, say PCP into a GC/MS it will certainly identify it as PCP, right?
Maybe, but often not!
When we were having trouble with decomposition of standards due to active sites in the GC system, we would inject a pure standard of PCP. (Yes, that PCP).
It's a useful diagnostic standard, and most productipn GC/MS labs keep it around (you can buy drugs of abuse as MS standards with no DEA license because they come in solutions of sample of such small quantity).
PCP is very prone to degrading in a GC column. Active sites can occur anywhere, but especially in the inject port (front end) and the transfer line to the mass spec ion source (back end).
In a properly functioning GC/MS, you would get a single peak, the spectra would be identified as PCP, the expected result. However if there were active sites in the injection port, the PCP would decompose into two compounds, which would then be separated by a number of minutes retention time, so the chromatogarm would show two distinct peaks (I can't remember the exact masses), neither of which was PCP. If the active sites were in the transfer line, the PCP would again decompose into two compounds but at the end of the column so you would only get one peak, but it was actually the two compounds co-eluting, and the mass spectra would again be characteristic not of PCP but the two decomposition products overlapped.
The moral of the story is that even when you know what you are dealing with a GC/MS is far from infallible, and as I have already mentioned it's not even applicable to many organic compounds.
You could try 4 more suitable extraction methods to get more information from the instrumental analysis - Soxhlet extraction of 3 different samples of the plant material with 1) Methanol 2) Hexane 3) Methylene Chloride and then analyzing each extract. The fourth extraction I would recommend is steam distillation.
You would almost certainly find out a lot more about the profile of compounds in the material by these extraction methods, but at the end of the day, it's an instrumental analysis, and one which may not even reveal the "active factors" at all, it's not magic and it cannot possibly provide you with enough information to be able to say "The active factor is X".
egor
Bluelighter
Hopefully there will be a few more tests in the coming weeks
Retired chemist, I sent the guy a pm with your suggestions for follow up testing, hopefully he will get back to me pretty quick
LuxEtVeritas
Bluelighter
MattPsy said:
HU210 IS is full agonist
THC is a partial agonist
Signal transduction studies have revealed that THC is actually a fairly weak partial agonist, according to Childers. The number of CB1 receptors in the brain is very large, comparable to the numbers of the monoamine receptors, such as those for serotonin and dopamine. This abundance of receptors, a phenomenon known as receptor reserve, explains how a partial agonist such as THC is able to produce a response. Basically, the more receptors in the system, the greater the likelihood of an agonist–receptor interaction. The presence of “spare receptors” (receptor reserve) increases sensitivity to an agonist, even a weak one such as THC.
kidamnesiac
Bluelighter
I believe the person running this GC/MS is a person who runs a shop and has a GC/MS in his garage. He has a picture of it on his website. It's not a student. Shame libraries are so expensive
Interesting info RC!
MattPsy
Bluelighter
LuxEtVeritas said:
Yeah I know dude, that's why I came to the conclusion I did. If it really were a full agonist (like if it contained HU210) then you'd expect the effects to be stronger than they are. Although, by making the amount they added low, you *could* only produce weak effects.
But if they DID add a full agonist like HU210 it'd be dangerous to sell because then if people took more than the recommended dose they could get seriously wasted off it, far more powerfully than with THC.
mad_scientist
Bluelighter
I was told (by someone who was selling Spice) that the active ingredient in Spice was the Pedicularis densiflora, but that rather than using simple dried plant matter, they actually added an extract from the P. densiflora onto the other plant ingredients.
We looked up P. densiflora and as far as I and the lady at the uni library could work out there has never been any proper analysis of what it might contain, so it would not surprise me if the Pedicularis species contain some novel CB1 agonist which has not yet been identified. Certainly smoking "Spice" produces a cannabis-like effect that is similar to, yet different from cannabis itself, so I would be surprised if it didn't contain a CB1 agonist of some sort, and it certainly doesn't contain THC as we had a sample analysed by the government drug lab.
On further research it appears that four species of Pedicularis are used in "herbal smoking blends" and teas and suchlike. We were not able to obtain P. densiflora as it was out of season, but I got some P. procera which I then did a solvent extraction on 50 grams of, and it did get me mildly stoned, not strong, but enough that I would be reluctant to dismiss it as placebo.
We had considered whether they might just be adding some kind of synthetic CB1 agonist, but which one? Not going to be HU210 as that stuff is way stronger and longer lasting than THC, feels more similar to a dissociative anaesthetic in effects than it does to THC. And while the effects of WIN55212-2 are mild and short lasting like Spice is, WIN55212-2 has a MW over 500, and decomposes if you try to smoke it. And CP55940 is pretty unstable, has to be shipped on ice and quickly goes off if stored at room temperature. So I am inclined to believe the Spice retailer that the active ingredient in Spice is indeed some kind of extract from P. densiflora, which must contain a novel CB1 agonist of which the structure has not yet been elucidated (although it appears that it dissolves in water, so is probably quite different to THC).
retired_chemist
Bluelighter
tobala said:
I had to look just out of curiosity. You can get a heap of scrap for thousand bucks. I bet the diff pump does not work, capacitors are shot, rods are probably covered in pump oil, and no doubt every ceramic in the rod assembly and ion source has been cracked from mismoving that old dog.
Oh, and there's no data aquisition system and no GC. LOL.
If it were in even some remote semblence of operational you can bet it would have been gifted to a small college for the tax write off.
LuxEtVeritas
Bluelighter
Is the effect undoubtedly even CB1 agonism of any nature or may it be some other pathway?
P. densiflora is known to be a tranquilizing and muscle relaxing herbal and such so perhaps maybe it is just standardized for a high concentration of those actives, but not a cannabinoid agonist.
egor
Bluelighter
I have seen a lot of info about pedicularis (densiflora, and several other species) being relaxing and tasting good to smoke, but never anything about a cannibis like stoning, even from the stronger extracts. Its fascinating if it really is responsible for the effects of these smoking blends though.
tobala said:
if it is on ebay it means that they haven't managed to sell it through normal channels, its sold as seen, which in turn means it probably doesn't work,
there are bargains to be had but not through ebay. Universities and companies sell off fully functional machines with a GC for no more than 3-7k USD.
The libraries of mass spectra are available free if you know where to look, the data will be in the format for HP chemstation or similar, but any reasonably competent coder would be able to convert the data to whatever program is being used. there are commercially available translators too. I have seen some older systems controlled by new bespoke software which is simpler to use than the current state of the art.
If spice is in fact Pedicularis densiflora or some other extract on an inert carrier it would explain how spice is available in such different strengths.
