So I had a wicked intense dream and I wrote it all down. Here it is:
There are many rumor's flying around about yellow spice, red spice, white spice, pink spice, purple spice, orange spice, upside down spice, sideways and backwards inside out spice. :shock: I think its time we settle the matter of whats the difference between the major forms of spice white, red, and yellow.
First what do I mean by white red and yellow spice. By white spice I mean recrystallized spice purified any number of ways but most commonly A/B and STB. It can be pure white crystals, clear crystals, or crystals with a yellow tinge. By yellow spice I mean an oily substance that is usually what is first obtained from an A/B or STB extract before cleaning it up or recrystallizing. It can also be obtained by evaporating the supernatant from for example from a hexane recrystallization. Others report other ways so please share them if you have them. By red spice I mean what is commonly referred to as jungle spice. This is obtained by A/B or STB but instead of using naptha, hexane, or heptane one uses toluene, xylene, or diethylether. The consistency of both red and yellow spice can vary from very oil and a liquid at room temperature to solid and sometimes even a bit crystalline.
So how do we go about solving this problem of whats in it and possibly why users report different types of experiences. We have the human side and the analytical side. Endlessness has already proposed a double blind protocol which is great. This discussion will focus on the analytical side and I encourage those who have experience with these forms to chime in with how they were prepared or how one can change between the different forms. There are also a number of threads that have touched upon this topic that I would recommend reading if your not familiar:
Experimental
Plant source: Mimosa hostillis
1mg/ml solutions in methanol of each form of spice was prepared. They were analyzed by LC-MS and GC-MS. LC-MS used a methanol water gradient (0.1% formic acid), C18 (reverse phase) column, UV wavelength 254 and 350n nanometers, and atmospheric pressure chemical ionization (scan range 50-1000 atomic mass units). I will skip over the rest of the details for now. They were also analyzed by GC-MS using single quadropole mass spec and chromatography took place in a typical methyl 5% phenyl polysiloxane capillary column. Again I will skip over the details for now but the injector temperature was 290 degrees C and the final oven temperature 300 degrees C.
The LC-MS didn't reveal much but it has certainly lent some important clues which will be useful. Basically the white spice had just dmt, the yellow and red spice had dmt + some impurity which would not ionize because of low concentration. The interesting detail is that the peak area which is a measure of the concentration differed a lot between the white spice and the red and yellow spice. The white spice hard a large peak for dmt and the other 2 had much smaller peaks. This means that the ratio of dmt to other stuff varies quite a lot between white spice and the other 2 forms. It also means that whatever it is it does not absorb UV light at 254 nanometers. If it were an indole alkaloid it would absorb light at 254 nanometers especially if it was in such a considerable concentration.
So this led me to take another look at these samples with GC-MS. Since each solution was in the same concentration I wanted to see again if the peak area for dmt differed. If all 3 solutions had the same amount of dmt you would expect the peak area to be similar and this is indeed what would happen if you injected the same sample over and over again. But again the peak area differed. White spice had the most and red and yellow had less. I will go into a bit more details here because I think its important.
The total ion count (TIC) for dmt in white spice was 86906703 for red spice 42133850 and yellow spice 50814225. So both the red and yellow spice contain about half as much dmt as the white spice. Note such as estimation is very rough and there are better ways to go about figuring that out which can be tried later if necessary. Regardless the ratios will certainly vary between samples depending on how they were prepared and the plant source.
The impurity profile is also interesting. Note that these impurities are only the volatile organic impurities. Anything that doesn't enter gas phase at 290 degrees C or breaks down at such temperatures will not be observed. White spice was about 98% pure. The major impurities appear to be n-methyl-tryptamine (NMT), 2-methyl-1,2,3,4-tetrahydro carbonline (THCB), an unknown and what appears to be a common contaminant that can come from certain plastics octadecenamide (can't say what isomer). I don't remembering using plastic but who knows these samples are quite old and they were stored in a glass container with a plastic lid so it could have leached from there. Maybe something with plastic was used in extraction procedure or the solvent itself was contaminated. I do not know if this compound is found in plants. Its found in mammals though and interacts with cannabinoid system. Of course the identification could also be incorrect without a reference to check it.
ANYWAY....red spice was about 97% dmt with pretty much exactly the same impurity profile as white. Yellow spice was about 90% dmt with the same impurities plus an additional impurities each about 1%. The two new impurities are a bit interesting as they somewhat resemble phenylethyl amines in their mass spectra such as n-methyl phenylethyl amine and dimethylphenylethyl amine. But again without a reference this cannot be confirmed. The other major impurity in yellow spice about 4% was NMT.
So what does all this mean and what can be done to figure more out? The presence of NMT and THCB both would make sense biosynthetically and I do believe NMT has been reported in mimosa hostillis. The phenyl ethyl amines may also make sense biosynthetically if whatever enzymes alkylates tryptamine can also alkylate (methylate) phenylethylamine. The other impurities I can't be sure about.
What is interesting however is that the volatile components are all very similar between the different kinds of spice. For some reason this batch of yellow spice has the most impurities and it would be interesting to see if that's often the case. But what accounts for the missing mass? If the amount of dmt in the yellow and red spice was truly about half (this measurement can be refined with a more quantitative comparison) then that is the other half? The impurities are not present in high enough concentrations to account for most of the mass. Based on previous data with trimethylsilyated derivitized red spice a fatty acid was detected but again it doesn't appear to be enough to account for the missing mass. There could of course be other fatty acids present and this would indeed make sense. It would be interesting to see if there were more or less fatty acids in defatted preparations versus non defatted.
HOWEVER it does seem that whatever these other impurities are 1- they are not a volatile indole alkaloid. In fact they are probably not an alkaloid at all because they also don't show up at 254 nanometers in LC chromatogram. However whatever it is it should be absorbing visible light otherwise it wouldn't have any color. There is a way to at least identify whether or not there is another impurity that could be separated and observed from the rest of the sample. A more universal detector like evaporative light scattering or thin layer chromatography with some different spray reagents should do the trick. Next time I remember a dream I will post about those experiments. NMR measurements of course would be the golden ticket to figuring this all out.
There are many rumor's flying around about yellow spice, red spice, white spice, pink spice, purple spice, orange spice, upside down spice, sideways and backwards inside out spice. :shock: I think its time we settle the matter of whats the difference between the major forms of spice white, red, and yellow.
First what do I mean by white red and yellow spice. By white spice I mean recrystallized spice purified any number of ways but most commonly A/B and STB. It can be pure white crystals, clear crystals, or crystals with a yellow tinge. By yellow spice I mean an oily substance that is usually what is first obtained from an A/B or STB extract before cleaning it up or recrystallizing. It can also be obtained by evaporating the supernatant from for example from a hexane recrystallization. Others report other ways so please share them if you have them. By red spice I mean what is commonly referred to as jungle spice. This is obtained by A/B or STB but instead of using naptha, hexane, or heptane one uses toluene, xylene, or diethylether. The consistency of both red and yellow spice can vary from very oil and a liquid at room temperature to solid and sometimes even a bit crystalline.
So how do we go about solving this problem of whats in it and possibly why users report different types of experiences. We have the human side and the analytical side. Endlessness has already proposed a double blind protocol which is great. This discussion will focus on the analytical side and I encourage those who have experience with these forms to chime in with how they were prepared or how one can change between the different forms. There are also a number of threads that have touched upon this topic that I would recommend reading if your not familiar:
Experimental
Plant source: Mimosa hostillis
1mg/ml solutions in methanol of each form of spice was prepared. They were analyzed by LC-MS and GC-MS. LC-MS used a methanol water gradient (0.1% formic acid), C18 (reverse phase) column, UV wavelength 254 and 350n nanometers, and atmospheric pressure chemical ionization (scan range 50-1000 atomic mass units). I will skip over the rest of the details for now. They were also analyzed by GC-MS using single quadropole mass spec and chromatography took place in a typical methyl 5% phenyl polysiloxane capillary column. Again I will skip over the details for now but the injector temperature was 290 degrees C and the final oven temperature 300 degrees C.
The LC-MS didn't reveal much but it has certainly lent some important clues which will be useful. Basically the white spice had just dmt, the yellow and red spice had dmt + some impurity which would not ionize because of low concentration. The interesting detail is that the peak area which is a measure of the concentration differed a lot between the white spice and the red and yellow spice. The white spice hard a large peak for dmt and the other 2 had much smaller peaks. This means that the ratio of dmt to other stuff varies quite a lot between white spice and the other 2 forms. It also means that whatever it is it does not absorb UV light at 254 nanometers. If it were an indole alkaloid it would absorb light at 254 nanometers especially if it was in such a considerable concentration.
So this led me to take another look at these samples with GC-MS. Since each solution was in the same concentration I wanted to see again if the peak area for dmt differed. If all 3 solutions had the same amount of dmt you would expect the peak area to be similar and this is indeed what would happen if you injected the same sample over and over again. But again the peak area differed. White spice had the most and red and yellow had less. I will go into a bit more details here because I think its important.
The total ion count (TIC) for dmt in white spice was 86906703 for red spice 42133850 and yellow spice 50814225. So both the red and yellow spice contain about half as much dmt as the white spice. Note such as estimation is very rough and there are better ways to go about figuring that out which can be tried later if necessary. Regardless the ratios will certainly vary between samples depending on how they were prepared and the plant source.
The impurity profile is also interesting. Note that these impurities are only the volatile organic impurities. Anything that doesn't enter gas phase at 290 degrees C or breaks down at such temperatures will not be observed. White spice was about 98% pure. The major impurities appear to be n-methyl-tryptamine (NMT), 2-methyl-1,2,3,4-tetrahydro carbonline (THCB), an unknown and what appears to be a common contaminant that can come from certain plastics octadecenamide (can't say what isomer). I don't remembering using plastic but who knows these samples are quite old and they were stored in a glass container with a plastic lid so it could have leached from there. Maybe something with plastic was used in extraction procedure or the solvent itself was contaminated. I do not know if this compound is found in plants. Its found in mammals though and interacts with cannabinoid system. Of course the identification could also be incorrect without a reference to check it.
ANYWAY....red spice was about 97% dmt with pretty much exactly the same impurity profile as white. Yellow spice was about 90% dmt with the same impurities plus an additional impurities each about 1%. The two new impurities are a bit interesting as they somewhat resemble phenylethyl amines in their mass spectra such as n-methyl phenylethyl amine and dimethylphenylethyl amine. But again without a reference this cannot be confirmed. The other major impurity in yellow spice about 4% was NMT.
So what does all this mean and what can be done to figure more out? The presence of NMT and THCB both would make sense biosynthetically and I do believe NMT has been reported in mimosa hostillis. The phenyl ethyl amines may also make sense biosynthetically if whatever enzymes alkylates tryptamine can also alkylate (methylate) phenylethylamine. The other impurities I can't be sure about.
What is interesting however is that the volatile components are all very similar between the different kinds of spice. For some reason this batch of yellow spice has the most impurities and it would be interesting to see if that's often the case. But what accounts for the missing mass? If the amount of dmt in the yellow and red spice was truly about half (this measurement can be refined with a more quantitative comparison) then that is the other half? The impurities are not present in high enough concentrations to account for most of the mass. Based on previous data with trimethylsilyated derivitized red spice a fatty acid was detected but again it doesn't appear to be enough to account for the missing mass. There could of course be other fatty acids present and this would indeed make sense. It would be interesting to see if there were more or less fatty acids in defatted preparations versus non defatted.
HOWEVER it does seem that whatever these other impurities are 1- they are not a volatile indole alkaloid. In fact they are probably not an alkaloid at all because they also don't show up at 254 nanometers in LC chromatogram. However whatever it is it should be absorbing visible light otherwise it wouldn't have any color. There is a way to at least identify whether or not there is another impurity that could be separated and observed from the rest of the sample. A more universal detector like evaporative light scattering or thin layer chromatography with some different spray reagents should do the trick. Next time I remember a dream I will post about those experiments. NMR measurements of course would be the golden ticket to figuring this all out.