Mass Spec Thread

[Dr JIM]

I just about to send my stuff for mass spec found a third party from a university lab willing to do the test. I pretended to be a grad student so if the testing goes well first time it will be worth and its a accredited lab too.. Sweet he even answered a purity question which hopefully helps
I can only make a rough estimate the purity of the compound based on the intensity of the LC-MS peak versus the TIC plot. The purity will be based exclusively on compounds which can be ionized by electrospray.

Why perform a test and produce results that have no basis in laboratory science.

Can you show me an analysis of this sort from a reputable lab? Does this "accredited lab" understand your intentions to use MS AUC (Area Under the Curve data) to determine 'purity"?

The fact is cutting corners to save money in the lab only diminishes the reliability and reproducibility of the results.

If you want purity data THAT IS USEFUL you MUST perform an LC OR GC guys, its that simple.

Moreover while I agree the MW data obtained in Daltons by MS is, or should be VERY accurate (about 0.01-0.02% of the compounds MW) it does not eliminate the possibility another compound of near identical MW has been detected (and substituted).

However there are other tests which can be used to determine whether the substance in question is a "sterol" molecule such as melting point and spectroscopy.


Regs
jim

 

[shamrockbear1]

Why perform a test and produce results that have no basis in laboratory science.

Can you show me an analysis of this sort from a reputable lab? Does this "accredited lab" understand your intentions to use MS AUC (Area Under the Curve data) to determine 'purity"?

The fact is cutting corners to save money in the lab only diminishes the reliability and reproducibility of the results.

If you want purity data THAT IS USEFUL you MUST perform an LC OR GC guys, its that simple.
Regs
jim

Thanks Dr. Jim I will relate it to the lab its a university lab so I think they decent they are a big 10 school so I think the equipment should be there they need. I'm new to testing so any advice to let them know would be great thanks

 

[Dr JIM]

Inform them you need BOTH an LC and a MS, to first determine the PURITY and second to establish the compounds MW.

Understand these two tests are almost always performed in "tandem" bc the LC enables the separation (and removal) of impurities from the parent molecule, the latter then being analyzed by MS thereafter.

Regs
jim

 

[Dr JIM]

The idea is to unequivocally establish the good labs from those that suck with reliable data. Do we really want tests performed that are going to be, and should be, challenged?

Damn I hope not bc then Meso will become known as the forum which posts UGL quality, purity, and concentration info on AAS products being sold, which is no better than data retrieved from a kindergartners chemistry set.

My point, do it right or don't do it at all.

Respects
jim

 

[devildog93]

Yes we do, or at least i do. Any data is more than we have. What else are we to do, take a source at his word...really?

 

[Dr JIM]

What are we to do? Take a sources word, HELL NO!

Simply perform the appropriate tests by ensuring they answer the questions your looking for on quality, purity, concentration, etc.

Oh and rest rest assured the fact one has "no data" is much better than acquiring the WRONG DATA!
regs
Jim

 

[beedix]

Any data is not good data. Agree with Jim on this.

This is actually positive news IMO. The results coming from these tests have not added up.

 

[devildog93]

Any data from MEMBERS I TRUST is good data to me. I trust a labmax done by someone who has done over 20 of them like i would trust someone's results off his 10th cycle of the same gear(long test esters for instance). People aren't going to stop buying and using while we wait for the golden lab to fall out of the sky. I would love to see purity numbers from the best lab we can find, but until then i will go with what we have.

 

[beedix]

I don't think it's a matter of a golden lab.

The results, if tested incorrectly, are meaningless.

Keep in mind the members you trust are not the ones qualified to operate sophisticated chemistry equipment. They are just shipping samples to someone else. It all the results are coming from someone without the appropriate experience, then.....

 

[devildog93]

I was talking more about labmax tests done by vets who know how to interpret the data. If we are talking about the mass specs done by Angus, then i would say i'm leaning towards their credibility although that is mainly colored by who leads attacks against them. I have had direct dealings with a couple of his attackers and know them to be selective scammers, so their credibility is shot with me.

 

[Dr JIM]

Any data from MEMBERS I TRUST is good data to me. I trust a labmax done by someone who has done over 20 of them like i would trust someone's results off his 10th cycle of the same gear(long test esters for instance). People aren't going to stop buying and using while we wait for the golden lab to fall out of the sky. I would love to see purity numbers from the best lab we can find, but until then i will go with what we have.

Yep haven't we heard the same argument for "trusting sources that we know". The FACT is many of the tests being performed do NOT meet the specifications required for the results achieved.

(Do understand I am NOT attacking ANYONE ON MESO on this issue! The truth of the matter is others have used junk science as a means to an ends, obtaining "reliable" quantitative and/or qualitative AAS analyses at a much cheaper price by ELIMINATING traditional labs standards. This is "bro science" pure and simple which has come to Meso to rest it's ugly arse.)

Here I'll type it one more time, purity and/or concentration results mandate the use of either a GS or LC it really is that rudimentary. Now that means ANY purity or concentration "estimates" achieved using MS ALONE are not even gross approximations, bc there is NO BASIS or standard for such an evaluation in laboratory science, period.

This MS-AUC "purity process" violates every well established lab standard on purity, quality and concentration, established by Phd and master degree chemists over several decades.

So if data on AAS is to be "published" make sure it's accurate or become the laughing stock of AAS boards.

AS I've said earlier the best LabMax tests can achieve is raising the probability the substance in question IS A STEROID. WHY? Because the UV absorbance shifts will only vary from 50-100 nm based on the different functional groups on each anabolic agent. What does that mean? A different shade of blue or green or perhaps orange IF it's a colorimetric assay as is LabMax. (LABMAX would be an excellent adjunct as proof the compound detected by MS is a steroid, rather than some other compound of similar Molecular Weight)

There are those who want to continue "as is" because "it's working", well to the contrary it's not working bc it's NOT evidence based, and THAT IS WHAT MAKES Meso Special!

Regs
jim

 

[flenser]

@Dr JIM, a failed labmax result accurately proves what's in the vial doesn't match what's on the label. Agree with the rest of your evaluation. A passing labmax result is not very useful.

 

[Dr JIM]

You got it!

It's quite sensitive yet also very nonspecific. Similar tests have been used for years as "screening tools" for competitive modern day athletes to determine if they have used ANY AAS.

Thus a negative result means the answer is an unequivocal NO, while a positive result mandates further testing, such as MS. Obviously the MS would confirm WHICH AAS was being used based on the metabolites detected in urine.

Regs
Jim

 

[Dr JIM]

I believe a few examples would help emphasize some points.

 

[Dr JIM]

Take a look at the UV spectra the primary difference the TREN absorbance peak is lowered because it has only 18 carbons (absent a methyl group) the absorbance shift is actually the result of an ALCOHOL (guess which one).

The spectra of Primo and TT are essentially identical because the combined number of C, OH, CH-3 are identical but their positions have changed.

Now to create a multi-peak spectra on LM or any other form of UV spectroscopy , just add a few contaminants and tada it's done!

Now understand because these different absorbance wavelengths typically correspond to a particular COLOR, when the sample is "pure", so is the color. However once ANY impurities make themselves into that sample, color shades (or an entirely different color) will begin to appear.

So there really are a variety of ways to delegitimize LM accuracy, but as Flenser said if the LM test is POSITIVE an AAS is present!

regs
jim

 

[Dr JIM]

Sorry Flenser I quoted us both INCORRECTLY, because a POSITIVE LM test could result thru the analysis of many compounds (and there are TENS of THOUSANDS) within the known AAS U.V. absorbance range.

HOWEVER a NEGATIVE LM test rules out the presence of ANY compound within that absorbance range INCLUDING AAS.

Sorry bout that F!

Regs
Jim

 

[flenser]

Sorry Flenser I quoted us both INCORRECTLY, because a POSITIVE LM test could result thru the analysis of many compounds (and there are TENS of THOUSANDS) within the known AAS U.V. absorbance range.

HOWEVER a NEGATIVE LM test rules out the presence of ANY compound within that absorbance range INCLUDING AAS.

Sorry bout that F!

Regs
Jim

Ah, that makes more sense. A while back a coworker listed some compounds that could possibly give a false positive on AAS colorimetric tests (not going to post them, of course). At the time I was asking why some AAS (like dbol) overpowered other AAS with much higher concentrations, but she didn't provide a good answer - at least not one I could understand.

 

[whwlives]

Here is a (slightly old) paper on the identification and analysis of steroids. FWIW, while GC/MS (and now LC/MS) ARE THE analytical "standard" a simple identification and a TLC plate WILL determine relative purity or impurity.

 

[whwlives]

To add to this, the analytical pharmacopeia standard for (example) testosterone enanthate doesn't even list GC, LC, or MS at all.

 

[Dr JIM]

To add to this, the analytical pharmacopeia standard for (example) testosterone enanthate doesn't even list GC, LC, or MS at all.

While I'll admit TLC is no doubt much better than LabMax it's cumbersome and somwhat limited in it's ability to eliminate high volumes of contaminants.

There is no doubt multiple TLC runs could accomplish the task currently being performed by HPLC, but the shear volume of contaminants seen in many UGL products limits their analyses to HPLC.

Moreover TLC has a HUGE learning curve bc different substances are best eluted using different solvents in both the stationary/ mobile phase AND thereafter the substance must be detected utilizing specialized forms of light.

For these reasons TLC has largely been replaced by HPLC.

Regs
Jim