Dr Jims Hplc/ms Data

[flenser]

FLENSER, I don't get involved in the explanation of the results anymore because I am not a chemist nor an expert. Even the most basic answers I am hesitant to answer because of the way that it gets twisted around. I am happy with helping someone out from time to time. That being said, I DID ask the dr at the University your question and his reply follows but I fear it is not as black and white as I had hoped it to be.

For that particular sample, the purity was low (29%), because many ions present (245, 397, 548, 700, 873, doubly charged and all related to each other) in abundant quantities that reduced ionization of 345 (Test Propionate), thus affect its purity estimation. These ions were not normally seen in the similar samples where we used them for reference, it must be something added other than the vegetable oils normally seen.
The concentration estimation was based on vegetable oil background for ionization from most other samples, so it was off, due to, the ionization competition in the electrospray, so that 76 mg/ml could be underestimate. Very likely, the manufacture did have 1 gram pure material dissolved in 10 mL solvent to make a 100mg/ml solution, but when it was analyzed by ESI, because of other ions in the solvent that are so much ionized, they reduced amount of Testosterone Propionate detected.
In short, our estimation can be affected by many variables, only when the variables are controlled (with reference compound, known amount in the same environment), then the estimation can be accurate.

Thanks, that actually answered two questions. The most important one being the concentration is an estimation of the raw powder rather than just the target hormone. Note that there are a LOT of people who believe the opposite, including sources using your services. An explanation on the summary page would be very useful.

 

[BigAngus]

It would seem to me that both scenarios can be true. There can be a high number of unknowns with the analyte or there can be a smaller than indicated amount of the analyte. Perhaps I can talk him into putting a blurb on the summary page about each one.

 

[Kinikuman]

because many ions present (245, 397, 548, 700, 873, doubly charged and all related to each other) in abundant quantities

I may be off but I think I have a broad idea what I think the additional substances are: ( a Benzamide ?, trifluoroacetates, trilinolenin)

 

[Dr JIM]

FLENSER, I don't get involved in the explanation of the results anymore because I am not a chemist nor an expert. Even the most basic answers I am hesitant to answer because of the way that it gets twisted around. I am happy with helping someone out from time to time. That being said, I DID ask the dr at the University your question and his reply follows but I fear it is not as black and white as I had hoped it to be.

For that particular sample, the purity was low (29%), because many ions present (245, 397, 548, 700, 873, doubly charged and all related to each other) in abundant quantities that reduced ionization of 345 (Test Propionate), thus affect its purity estimation. These ions were not normally seen in the similar samples where we used them for reference, it must be something added other than the vegetable oils normally seen.
The concentration estimation was based on vegetable oil background for ionization from most other samples, so it was off, due to, the ionization competition in the electrospray, so that 76 mg/ml could be underestimate. Very likely, the manufacture did have 1 gram pure material dissolved in 10 mL solvent to make a 100mg/ml solution, but when it was analyzed by ESI, because of other ions in the solvent that are so much ionized, they reduced amount of Testosterone Propionate detected.
In short, our estimation can be affected by many variables, only when the variables are controlled (with reference compound, known amount in the same environment), then the estimation can be accurate.

Angus do you have any idea what happens to an MS when oils are significant component of injected material?

The same is true of an HPLC unless …..
Want a hint? How much did the involved MS cost ….. unless

 

[MANWHORE]

What is the chemical analysis required, by the FDA

 

[Dr JIM]

Generally both HPLC and MS are needed,

However these requirements may vary considerably for those substances intended for human consumption and/or whether it's being marketed as a "supplement" or pharmaceutical, the latter requiring a prescription.

To that end "medications" which require an RX will also require a MS and HPLC, especially for introductory medications, in addition to clinical trials.

 

[Kinikuman]

To that end "medications" which require an RX will also require a MS and HPLC, especially for introductory medications, in addition to clinical trials.

This is absolutely correct. In fact, at each step of the synthesis (not just the end product) of any compound, data would need to be provided that verified acceptable purity levels on a batch level basis before it can introduced into any organism for either scientific research or medical purposes. QC processes such as these are why you can analyze 10K pcs. of Bayer Aspirin @ 500mg. and they will meet an incredibly high and uniform degree of purity and accuracy of dosage.

 

[REF]

I am ready to see some tests. Thanks for doing this and I also thank angus for doing what he could to try and help his fellow bro,s . I think all of this is good for the community but im sure some srs will be upset and have lots of excuses.

 

[BigAngus]

I am ready to see some tests. Thanks for doing this and I also thank angus for doing what he could to try and help his fellow bro,s . I think all of this is good for the community but im sure some srs will be upset and have lots of excuses.

Thanks bro, i think that, at the end of the day, Jim and I have the same intentions, but just very different ways of expressing them and enacting them.

 

[WMSuperSport]

Yeah I think we all want quality product. I have faith that through all this hard work you guys are doing, ends with our community being much more informed and hopefully safer. Thanks to you guys

 

[Dr JIM]

Well it seems we have wasted enough time on whether Methanol is an "appropriate solvent" for AAS. But crap it seems the chemist used the "wrong solvent" in this case also. I wonder why that is? Because it's NOT the wrong damn solvent, duh

 

[Dr JIM]

This was one of the earlier samples I had analyzed. Notice the procedural discussion with the inclusion of the TT calibration curve.

The CC is now stored in the HPLCs databank and may be used for upcoming Testosterone analyses. However after several weeks to months of use the INHERENT HPLC parameters may change and the CC will need to be repeated to ensure accuracy.

This "recalibration effect" is one of many reasons why the Testosterone elution peaks occur at different timed intervals compared to some of the earlier HPLC studies I've posted in this thread.

 

[CensoredBoardsSuck]

Well it seems we have wasted enough time on whether Methanol is an "appropriate solvent" for AAS. But crap it seems the chemist used the "wrong solvent" in this case also. I wonder why that is? Because it's NOT the wrong damn solvent, duh

Do you want me to PM Regular and get him to come take a look at it? LMFAO

 

[Dr JIM]

Well maybe we should wait until I receive the next THIRD set of analyses. Surely no chemist would not make such an egregious error (using methanol) if given a third shot!

However should this happen again, we must assume my chemist is "on drugs" and insist some pharmacopeia toting HPLC expert from TID, like Regular, conduct the remaining analyses.

 

[Dr JIM]

Ok I hope folks now understand WHY you just can't gander at an HPLC and determine the relative concentrations of compounds. (A process often used by OL labs to exaggerate their AAS content.

While it's true an approximation may be made using the AUG percentages the Calibration Curve data MUST be appropriately integrated into a conventional HPLC AUG formula.

Hey notice that double peak in the HPLC above? Take a close look and you will see there is a "technical" error. Look at how the total testosterone concentration. How was it derived, using BOTH peaks, OOPS!

Thats the error! There are a few exceptions but the summation of peaks is rarely appropriate to determine a substances concentration.

So the concentration of this particular PRIVATE LAB testosterone product is ~ 150mg/ml

NOW there is something else here that emphasizes an earlier point. The UVa absorption scale MUST be show as a qualitative value rather than a percentage of absorption. Otherwise the values are EASILY manipulated using simple "tricks" such as constraining the elution times or coning in on a particular peak.

 

[flenser]

Hey notice that double peak in the HPLC above? Take a close look and you will see there is a "technical" error. Look at how the total testosterone concentration. How was it derived, using BOTH peaks, OOPS!

From the first page I got the impression the concentration was of "Unknown Steroids" which included both peaks. I don't see where either peak is positively identified as testosterone?

 

[Dr JIM]

Actually "unknown steroid" is a notation the chemist uses as a reminder of what the sample should contain.

 

[Dr JIM]

You know what that's a good point. The substance being investigated is labeled as testosterone in the calibration curve. What should have been included (and was at the the begining of this 4 sample set) to reveal the sample WAS indeed testosterone?

It's included in the earlier studies Ive posted.

Yet I've NEVER seen it included by HPLCs conducted by OL labs, NEVER!

 

[MANWHORE]

Switch up that avatar Brother Jim.
That chick's tits are getting old. Try a nice ass

 

[Dr JIM]

Oh no its KING KONG I enjoy so much
Besides I dont believe I could ever run from those boobs.
Her ass is very nice too hmmm,,,,

The problem, you find her and you may find me!