You should try UGBB if you do let me know I would love seeing what happens ahahha
MESO-Rx
Anabolic Steroids
Readalots Enhanced Testing
- Thread starter Dirthand
- Start date
readalot
Member
They would not let me in. Denied my registration multiple times.
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.
readalot
Member
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.
What would be grounds for denying someone's registration?
Do they think you are under age, lol?
Or they know you got banned somewhere else.
readalot
Member
Insert shrug emoji.
readalot
Member
I appreciate your consistent support @Vanargandar. Thanks very much for your effort. Really nice of you.
And of course @iris. A rock. Thank you very much.
And of course @iris. A rock. Thank you very much.
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readalot
Member
I know your busy @janoshik. Look forward to your comments on this. Thanks.Thanks for the comments.
So we are back to this:
TE:
Delta-6 TE:
That alkane in TE at C(6)-C(7) ain't budging at room temperature or at any temp your car may reach on a hot day. Shows the raws manufacturer doesn't care or clueless.
This impurity would only be formed during synthesis step.
Dehydrogenation - Wikipedia
en.m.wikipedia.org
can you detect this impurity with your standard HPLC method?
Funny that you ask, just today I've detected that, what I also believe to be delta 6 variant, in test cyp raws when I ran the test out of my personal curiosity!
(ignore the autoassigned name for the impurity)
I mean, what else would Jano do over the weekend, right?
It IS allowed in...
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.
readalot
Member
This too. Not clear to me if your HPLC method as is can discern -ene (missing one H) impurities from test ester.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?
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.
janoshik
Subscriber
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?
Okay, I'm lying. It was yesterday.
This is actually the most important find (well, re-find) of this project, so I thought it might deserve some additional investigation.
readalot
Member
readalot
Member
- potential impurity list seems limited.
- no thermal degradation of Test Cyp after 48 hr at 80 deg C.
Of course this temp lower than typical GC temp ramp.
This paper suggests creation of minor thermal impurities with GC-FID.
Didn't pull the whole paper.
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readalot
Member
Structural Insights and Intermolecular Energy for Some Medium and Long-Chain Testosterone Esters
Testosterone (17β-Hydroxyandrost-4-en-3-one) is the primary male anabolic-androgenic steroid. The crystal structures of two medium and two long esterified forms of testosterone, including enanthate, cypionate, decanoate and undecanoate, were determined by X-ray single crystal diffraction. The...
www.mdpi.com
both Test Cyp and Test E rock solid stable up to 300 deg C in nitrogen blanket.
Fig. S5 from supplemental material.
janoshik
Subscriber
That's a good find.Structural Insights and Intermolecular Energy for Some Medium and Long-Chain Testosterone Esters
Testosterone (17β-Hydroxyandrost-4-en-3-one) is the primary male anabolic-androgenic steroid. The crystal structures of two medium and two long esterified forms of testosterone, including enanthate, cypionate, decanoate and undecanoate, were determined by X-ray single crystal diffraction. The...
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
readalot
Member
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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janoshik
Subscriber
Mostly 350C.
Testosterone really hates being a gas.
Testosterone really hates being a gas.
readalot
Member
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!!
janoshik
Subscriber
I use higher temps for quite important reasons 
Cheers
Cheers
readalot
Member
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).
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Using Comprehensive GC×GC–TOF-MS for Enhanced Detection and Separation in Antidoping Control Screening
The misuse of androgenic anabolic steroids in sports was banned in 1976 by the International Olympic Committee and global sports community. The illegal use of anabolic steroids has reached disturbing levels worldwide. This worldwide problem is fueled partially by an ever-increasing demand for...
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.
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https://www.waters.com/content/dam/waters/en/app-notes/2007/720002251/720002251-ja.pdf
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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(PDF) Thermal stability evaluation of doping compounds before GC-MS analysis by DSC
PDF | The Medical Commission of the International Olympic Committee forbids the use of anabolic androgenic steroids, β-agonists, stimulant and narcotic... | Find, read and cite all the research you need on ResearchGate
www.researchgate.net
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BigNoOne
New Member
How are compounds tested for purity that go to the compounding pharmacies. Do the same.
It’s HPLC testing.
