HPLC-MS or GC-MS analysis

[mtf]

Hello.

Does any testing laboratory offers high pressure liquid chromotography-mass spectrometry or gas chromatography-mass spectrometry? I am interested in compound identification and quantitative analysis of impurities of small molecules (< 1 000 Da).

 

[Bearslovecheese]

Your only hope in this neck of the woods is @“Janoshik” for testing.

 

[mtf]

Bearslovecheese" pid='13955' dateline='1526747518:

Your only hope in this neck of the woods is @“Janoshik” for testing.

Unfortunately, Janoshik is known to not to disclose relevant facts to the customers, as in https://thinksteroids.com/community...n-and-liar-thread-you-be-the-judge.134381544/. I am agnostic as to whether he actually tested the substance in this case. The lack of professionalism on the other hand, is undeniable. The raw data he provides is of no use without calibration data. I have enough education in chemistry to know that the test he does of HPLC-UV detector is very unspecific and moreover highly dependent on the experimental setup (eluent, eluent gradient, column material, and pumping rate). Basically he guesses the compound based on retention time (it is impossible to identify it because many compounds will have the same retention time for any chromatography setup). At least a simple UV-vis spectrogram of the most abundant fraction would make it credible, but he does not even do that. Melting point determination, used as a “sanity check”, is a must, but again he does not do that. I checked his sample raw data and noticed he does not even tell the aforementioned information, making his “raw data” useless. This service is a joke, and given the amount of guesswork involved, you could do thin layer chromatography (very cheap) in your house for a similar (uncertain) result.

 

[Janoshik]

mtf" pid='13959' dateline='1526749574:

Bearslovecheese" pid='13955' dateline='1526747518:

Your only hope in this neck of the woods is @“Janoshik” for testing.

Unfortunately, Janoshik is known to not to disclose relevant facts to the customers, as in https://thinksteroids.com/community...n-and-liar-thread-you-be-the-judge.134381544/. I am agnostic as to whether he actually tested the substance in this case. The lack of professionalism on the other hand, is undeniable. The raw data he provides is of no use without calibration data. I have enough education in chemistry to know that the test he does of HPLC-UV detector is very unspecific and moreover highly dependent on the experimental setup (eluent, eluent gradient, column material, and pumping rate). Basically he guesses the compound based on retention time (it is impossible to identify it because many compounds will have the same retention time for any chromatography setup). At least a simple UV-vis spectrogram of the most abundant fraction would make it credible, but he does not even do that. Melting point determination, used as a “sanity check”, is a must, but again he does not do that. I checked his sample raw data and noticed he does not even tell the aforementioned information, making his “raw data” useless. This service is a joke, and given the amount of guesswork involved, you could do thin layer chromatography (very cheap) in your house for a similar (uncertain) result.

Thank you for your educated opinion.

We’d appreciate if you wrote about your concerns to the people standing past US Pharmacopoeia and tell them that their methods are a joke and guesswork.

My RP-HPLC method is improved method from US Pharmacopoeia http://www.pharmacopeia.cn/v29240/usp29nf24s0_m77490.html

We’d be also very happy had you demonstrated a thin layer chromatography of the said substance with data output similar in quality to the method used in USP or my method.
We are sure people all around the world would appreciate it as then they wouldn’t have to buy machines worth tens of thousands $, instead just a few cheap plates.

Oh, and please, make a video of the melting point ‘sanity check’ on human growth hormone - it would provide quite some entertainment for everybody here.

Sanity check indeed.

We wish you the best of luck in finding a service satisfying your requirements.

 

[mtf]

Janoshik, your reply confirms my impression of your lack of professionalism by using sarcasm and a straw man fallacy to dodge sound criticism with pseudo-corporate language to hide the sarcasm.

All you wrote is irrelevant because you replied in the context of analysis of samples suspected to contain HGH. Since the original post I mentioned this is about small molecules so the methods specific for proteins and peptides is irrelevant.
mtf" pid='13825' dateline='1526652001:

I am interested in compound identification and quantitative analysis of impurities of small molecules (< 1 000 Da).

The fact is, you do not do even do MP determination for those compounds for which it can be done (like steroids) and you do not provide eluent, static phase and pumping rate information, making your “raw” data useless for your clients.
Janoshik" pid='14017' dateline='1526808601:

My RP-HPLC method is improved method from US Pharmacopoeia http://www.pharmacopeia.cn/v29240/usp29nf24s0_m77490.html

In what regards to your testing of HGH (which is not of interest to me, but you are using it as a distraction from my critique): I see you either did not even read your own link, or you think of your own clients as stupids who do not even know what proteases are. Either way it is a pity and a further reason for not to trust you. The USP method you linked uses chromatography with UV detection after cleavage with a protease (trypsin). From your http://janoshik.com/sample-raw raw data most of the area under curve is in single high peak, indicating you missed the crucial step of proteolysis. If you had performed proteolysis, you would have a rich spectrum where each fragment is visible as one peak. Without this, you are going to get a false positive for any long protein with roughly the same retention time as your reference HGH for your undisclosed eluents in your undisclosed column material, even if it is biologically inactive or something completely different from HGH.

So much for “improvement over the USP method”. Actually it is a cheaper (since you need not buy the protease) and far much less selective method (for the reason already described).

 

[Septicanon]

Anyone with half a brain knows something smells off with Janoshik’s testing ever since the Meso thing. The fact he goes full defensive/deflects when questioned further adds to that. Anyway… @“mtf” Simec is probably your best option but its expensive.

 

[Janoshik]

mtf" pid='14029' dateline='1526830834:

Janoshik, your reply confirms my impression of your lack of professionalism by using sarcasm and a straw man fallacy to dodge sound criticism with pseudo-corporate language to hide the sarcasm.

All you wrote is irrelevant because you replied in the context of analysis of samples suspected to contain HGH. Since the original post I mentioned this is about small molecules so the methods specific for proteins and peptides is irrelevant.
mtf" pid='13825' dateline='1526652001:

I am interested in compound identification and quantitative analysis of impurities of small molecules (< 1 000 Da).

The fact is, you do not do even do MP determination for those compounds for which it can be done (like steroids) and you do not provide eluent, static phase and pumping rate information, making your “raw” data useless for your clients.
Janoshik" pid='14017' dateline='1526808601:

My RP-HPLC method is improved method from US Pharmacopoeia http://www.pharmacopeia.cn/v29240/usp29nf24s0_m77490.html

In what regards to your testing of HGH (which is not of interest to me, but you are using it as a distraction from my critique): I see you either did not even read your own link, or you think of your own clients as stupids who do not even know what proteases are. Either way it is a pity and a further reason for not to trust you. The USP method you linked uses chromatography with UV detection after cleavage with a protease (trypsin). From your http://janoshik.com/sample-raw raw data most of the area under curve is in single high peak, indicating you missed the crucial step of proteolysis. If you had performed proteolysis, you would have a rich spectrum where each fragment is visible as one peak. Without this, you are going to get a false positive for any long protein with roughly the same retention time as your reference HGH for your undisclosed eluents in your undisclosed column material, even if it is biologically inactive or something completely different from HGH.

So much for “improvement over the USP method”. Actually it is a cheaper (since you need not buy the protease) and far much less selective method (for the reason already described).

Oh lord.

The peptide mapping is a different test from chromatographic purity. And you tell me to read it?

Try pressing CTRL+F and enter “chromatographic purity.”

You might know what a protease is, but you appear to be stupid enough to not realize it’s a different test from USP, where there are multiple different assays described.

Also, feel free to prove me wrong with DATA, instead or empty words, and show me a protein, which coelutes with HGH in both SEC and RP-HPLC assay with the same 214/280 nm absorbance ratio.

Until then don’t waste my time.

---

Septicanon" pid='14037' dateline='1526834818:

Anyone with half a brain knows something smells off with Janoshik’s testing ever since the Meso thing. The fact he goes full defensive/deflects when questioned further adds to that. Anyway… @“mtf” Simec is probably your best option but its expensive.

SIMEC also identifies compounds in the absolutely same manner as I do and our little chemist here doesn’t like that.

But I guess SIMEC is wrong as well

 

[DNPstoney]

Janoshik" pid='14043' dateline='1526839541:

mtf" pid='14029' dateline='1526830834:

Janoshik, your reply confirms my impression of your lack of professionalism by using sarcasm and a straw man fallacy to dodge sound criticism with pseudo-corporate language to hide the sarcasm.

All you wrote is irrelevant because you replied in the context of analysis of samples suspected to contain HGH. Since the original post I mentioned this is about small molecules so the methods specific for proteins and peptides is irrelevant.
mtf" pid='13825' dateline='1526652001:

I am interested in compound identification and quantitative analysis of impurities of small molecules (< 1 000 Da).

The fact is, you do not do even do MP determination for those compounds for which it can be done (like steroids) and you do not provide eluent, static phase and pumping rate information, making your “raw” data useless for your clients.
Janoshik" pid='14017' dateline='1526808601:

My RP-HPLC method is improved method from US Pharmacopoeia http://www.pharmacopeia.cn/v29240/usp29nf24s0_m77490.html

In what regards to your testing of HGH (which is not of interest to me, but you are using it as a distraction from my critique): I see you either did not even read your own link, or you think of your own clients as stupids who do not even know what proteases are. Either way it is a pity and a further reason for not to trust you. The USP method you linked uses chromatography with UV detection after cleavage with a protease (trypsin). From your http://janoshik.com/sample-raw raw data most of the area under curve is in single high peak, indicating you missed the crucial step of proteolysis. If you had performed proteolysis, you would have a rich spectrum where each fragment is visible as one peak. Without this, you are going to get a false positive for any long protein with roughly the same retention time as your reference HGH for your undisclosed eluents in your undisclosed column material, even if it is biologically inactive or something completely different from HGH.

So much for “improvement over the USP method”. Actually it is a cheaper (since you need not buy the protease) and far much less selective method (for the reason already described).

Oh lord.

The peptide mapping is a different test from chromatographic purity. And you tell me to read it?

Try pressing CTRL+F and enter “chromatographic purity.”

You might know what a protease is, but you appear to be stupid enough to not realize it’s a different test from USP, where there are multiple different assays described.

Also, feel free to prove me wrong with DATA, instead or empty words, and show me a protein, which coelutes with HGH in both SEC and RP-HPLC assay with the same 214/280 nm absorbance ratio.

Until then don’t waste my time.

---

Septicanon" pid='14037' dateline='1526834818:

Anyone with half a brain knows something smells off with Janoshik’s testing ever since the Meso thing. The fact he goes full defensive/deflects when questioned further adds to that. Anyway… @“mtf” Simec is probably your best option but its expensive.

SIMEC also identifies compounds in the absolutely same manner as I do and our little chemist here doesn’t like that.

But I guess SIMEC is wrong as well

---

The musings of a true professional and businessman!

 

[Janoshik]

ryantheco" pid='14054' dateline='1526853246:

The musings of a true professional and businessman!

If you want pretty words and correct phrases, then I believe the email was [email protected]

Suit yourself.

 

[Bearslovecheese]

Reading through this thread has my brain screaming set up. I got to finally read through the customs mishap people keep throwing Jano under the bus for, at least. I’m not here to beat dead horses. I’m not here to defend Jano, either - he’s capable of doing that himself. I don’t think you get to attack him repeatedly then bitch because his responses are crisp and curt though.

Mtf, good luck in finding the testing you’re looking for. I hope you are able to help your community in regards to raws/self-brewing/sourcing ready product in some way.

 

[Janoshik]

Bearslovecheese" pid='14087' dateline='1526873612:

Reading through this thread has my brain screaming set up. I got to finally read through the customs mishap people keep throwing Jano under the bus for, at least. I’m not here to beat dead horses. I’m not here to defend Jano, either - he’s capable of doing that himself. I don’t think you get to attack him repeatedly then bitch because his responses are crisp and curt though.

Mtf, good luck in finding the testing you’re looking for. I hope you are able to help your community in regards to raws/self-brewing/sourcing ready product in some way.

I agree with you.

I’ve seen this thread before you mentioned me and I had alarm bells ringing, so I didn’t reply.
Linking a link, which was never ever linked on this forum, only in a picture sent to EC in email when uncovering their fraud is a very interesting thing to do.
Especially linked with a nonsensical overly specific request (you can’t do quantitative or even semiquantitative analysis of impurities with mass spectrometer without standards - standards for all impurities would cost think like 200$ per impurity and mass spec would detect dozens of them).

Thank you and have a nice day.

 

[mtf]

Bearslovecheese" pid='14087' dateline='1526873612:

Mtf, good luck in finding the testing you’re looking for. I hope you are able to help your community in regards to raws/self-brewing/sourcing ready product in some way.

It is a problem of education. Many people do not know about raws. I have posted about it in some forums but also I encourage vendors that sell female hormones to search for transsexual forums and post there; they get more sales and the customers get a less expensive and more flexible product (e.g. long esters of estradiol are hard to find) so everybody wins.

 

[Sasquatch_Labs]

Analyzer from Meso has a solid reputation.

[email protected]

Jay

 

[Checkmatelabs]

Sasquatch Labs" pid='14888' dateline='1527438326:

Analyzer from Meso has a solid reputation.

[email protected]

Jay

DO NOT GO THROUGH ANALYZER.

ANALYZER WAS BUSTED A FEW WEEKS BACK. THERE ARE THREADS ALL OVER MESO ABOUT IT.

REPEAT: DO NOT GO THROUGH ANALYZER

 

[Atexus]

Sasquatch Labs" pid='14888' dateline='1527438326:

Analyzer from Meso has a solid reputation.

[email protected]

Jay

Yeah, there are articles in a Czech paper about him being a university student busted for testing drugs for americans

 

[Sasquatch_Labs]

Checkmatelabs" pid='14894' dateline='1527440919:

Sasquatch Labs" pid='14888' dateline='1527438326:

Analyzer from Meso has a solid reputation.

[email protected]

Jay

DO NOT GO THROUGH ANALYZER.

ANALYZER WAS BUSTED A FEW WEEKS BACK. THERE ARE THREADS ALL OVER MESO ABOUT IT.

REPEAT: DO NOT GO THROUGH ANALYZER

Had*

Just heard about it since I was gone. I deleted my comment.
Please disregard.

Jay

 

[mtf]

Bump.