Readalots Enhanced Testing

Thanks very much for taking the time to share that. It's the love of learning and feedback like yours that makes all this work worthwhile. I appreciate it.



That is a useful data point. I didn't know I had an
impersonator (?).

In my time I have been on TNation (banned twice and now on "mute"), ExcelMale (banned), MesoRx (still here), SST (still there), and ProMuscle (don't post, what's the point? LoL).

So I wouldn't say a ton. The first two aren't source forums. If there are other ones I am on please let me know haha.

Take care.
You should try UGBB if you do let me know I would love seeing what happens ahahha
 
Thanks very much for taking the time to share that. It's the love of learning and feedback like yours that makes all this work worthwhile. I appreciate it.



That is a useful data point. I didn't know I had an
impersonator (?).

In my time I have been on TNation (banned twice and now on "mute"), ExcelMale (banned x 3 or 4), MesoRx (2x soft ban, still here), SST (still there), and ProMuscle (don't post, what's the point? LoL).

So I wouldn't say a ton. The first two aren't source forums. If there are other ones I am on please let me know haha.

Take care.
My bad, I worded that oddly saw you in sponsored threads of the underground forum at Meso, not an entirely different forum. I'm going to take a chance on one of the vendors might submit to jano for some labs of my own.
 
My bad, I worded that oddly saw you in sponsored threads of the underground forum at Meso, not an entirely different forum. I'm going to take a chance on one of the vendors might submit to jano for some labs of my own.
Hey, cool. Thanks for clarifying. I'm hopeful I will make my first UGL purchase too in the near future! I mean really i already (unofficially) did buying from compounding pharmacies lol.
Best wishes on your journey. Take care.
 
Thanks for the comments.

So we are back to this:

can you detect this impurity with your standard HPLC method?



As always, I appreciate and admire your scientific curiosity and willingness to discuss all these intricacies. It's the weekend after all. Well done!

Great question whether these alkene variants of Test Cyp/Enan (USP testosterone impurities, etc) are typically counted in the Test Cyp/Enan pile for HPLC.
I know your busy @janoshik. Look forward to your comments on this. Thanks.
 
For comparison...



View attachment 302164

View attachment 302166


Would be funny if in a few months everyone wants to join the class action lawsuit against the AAS suppliers wanting a refund on that 10-20% of the their test ester they thought they were getting but weren't.

200 mg/ml [Test Cyp | Test E] becomes 160-180 mg/ml. With API concentration in play, that would get folks attention again. I look forward to learning more.

And that pharma COA one more time:




See those testosterone impurity values?
This too. Not clear to me if your HPLC method as is can discern -ene (missing one H) impurities from test ester.

Thanks @janoshik.

Which purity above is closer to reality? GCMS or HPLC? I didn't see you consider the heat induced dehydrogenation possibility for the delta-6 TE example.

Good stuff.
 
This too. Not clear to me if your HPLC method as is can discern -ene (missing one H) impurities from test ester.
I don't think so. I think it's two H's though.

Two carbons have to loose one to free themselves up for the loving embrace of a double bond.
Which purity above is closer to reality? GCMS or HPLC?
Impossible to tell without running GCMS on the reference standard as well.
I didn't see you consider the heat induced dehydrogenation possibility for the delta-6 TE example.
Not entirely confident I did.

But guess what I just did?

1731357625790.webp

Okay, I'm lying. It was yesterday.

1731357651995.webp


This is actually the most important find (well, re-find) of this project, so I thought it might deserve some additional investigation.
 
I don't think so. I think it's two H's though.

Two carbons have to loose one to free themselves up for the loving embrace of a double bond.

Impossible to tell without running GCMS on the reference standard as well.

Not entirely confident I did.

But guess what I just did?

View attachment 302428

Okay, I'm lying. It was yesterday.

View attachment 302429


This is actually the most important find (well, re-find) of this project, so I thought it might deserve some additional investigation.
Absolutely right, one proton per C atom.

Very cool. Thanks for ordering that!
 

both Test Cyp and Test E rock solid stable up to 300 deg C in nitrogen blanket.

With the increase in temperature, no thermal events occurred until the onset temperature of 320 °C for long esters (TDec, TUnd) and up to 350 °C for medium esters (TEna, TCyp).


3.7. Differential Thermal Analysis (DTA) and Thermogravimetric Analysis (TG)

DTA/TGA measurements were performed with a simultaneous thermogravimetric and differential thermal analyzer Shimadzu DTG-60H. The samples were heated with a heating rate of 10°C/min, using an alumina sample cell (diameter 5.8 × 2.5 mm2) under a dry nitrogen purge (70 mL/min).

Fig. S5 from supplemental material.
Figure S5.webp
 

both Test Cyp and Test E rock solid stable up to 300 deg C in nitrogen blanket.






Fig. S5 from supplemental material.
View attachment 302465
That's a good find.
 
That's a good find.
Appreciate it and my pleasure.

My hypothesis is the Test E reference standard will come through GCMS 99%+ unscathed. I don't think the vast majority of structural impurities detected in the Test ester raws are an artifact of the GCMS measurement. They are present in the raw.

What's your temperature program on the GCMS? 180 to 300 deg C range?
 
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Mostly 350C.

Testosterone really hates being a gas.
Whoa. This could get interesting. I thought most GCMS temp ramps for AAS were between 180 to 300 C aka non destructive. Thanks for the info. You may need to lower the max temp.

But good to see what your baseline analysis reveals for current temp ramp in house.

Thank you!!
 

Instrumentation
The GC/EI-MS/MS was performed using Agilent 7000 Series Triple Quadrupole GC/MS.

The GC system was equipped with the GC HP Ultra 1 column (21 m, i.d. 0, 2 m, film thickness 0.1 µm). A volume of 2 µl of the sample was injected in the GC system wich was operated in the split (15.8:1) mode. The GC oven temperature program started at 186C, was increased at 2C /min to 240C, followed by 22C/min to 320 C using helium as carrier gas (0.8 ml/min constant pressure). The injector and interface temperatures were set to 300C and the ion source was operated at 230C, electron ionization (EI) was used (70 eV).


==========


The helium carrier gas flow rate was set to 1.5 mL/min at a corrected constant flow via pressure ramps. The primary column was programmed with an initial temperature of 140 °C for 0.20 min then ramped at 20 °C/min to 170 °C, next ramped at 5 °C/min to 260 °C for 2.0 min, with a final ramp at 10 °C/min to 315 °C for 12.0 min. The secondary column temperature program was set to an initial temperature of 145 °C for 0.20 min then ramped at 20 °C/min to 175 °C, next ramped at 5 °C/min to 265 °C for 2.0 min, with a final ramp at 10 °C/min to 320 °C for 12.0 min.

=======



Anabolic Steroid Esters Extraction

A 100 mg of decontamined hair was incubated overnight at 50 °C in 1 mL MeOH in presence of 2 ng
testosterone-d3 and nandrolone-d3. After incubation, methanol was evaporated to dryness. The residue was reconstituted in 3 mL of 1 M phosphate buffer (pH 7.0). As anabolic steroids, extraction was made with C18 based SPE cartridges. The eluent was evaporated to dryness, and the residue reconstituted in 0.5 mL of 1 M phosphate buffer (pH 7.0). A further purification step was achieved by addition of 4 mL of hexane-ethyl
acetate (70:30, v/v). After agitation and centrifugation, the organic phase was removed and evaporated to
dryness. The residue was derivatized by adding 5 μL MSTFA-NH4I- 2-mercaptoethanol (250 μL, 5 mg, 15 μL respectively) and 45 μL MSTFA, then incubated for 20 min at 60 °C.


GC method
The samples were injected by splitless injection (1 μL, 270 °C, purge at 50 mL/min after 1 min) into a carrier gas of helium at a constant flow rate of 1.2 mL/min delivered from an Agilent 6890 GC. The column was an Ohio Valley OV 30m x 0.25 mm i.d., 0.25μm. The following temperature ramp rate was used: 60 to 325 °C (5 min) at 20 °C/min. The total run time was 18.25 min


=======

 
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Appreciate it and my pleasure.

My hypothesis is the Test E reference standard will come through GCMS 99%+ unscathed. I don't think the vast majority of structural impurities detected in the Test ester raws are an artifact of the GCMS measurement. They are present in the raw.

What's your temperature program on the GCMS? 180 to 300 deg C range?
How are compounds tested for purity that go to the compounding pharmacies. Do the same.

It’s HPLC testing.
 
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