angus's picture
angus
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+ 5 Estimation of Steroids Concentration by Mass Spec

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This was written by the dr and seems like an excellent time to post it, it describes how the ion count (which is what he uses) is the same as using the peak method that is common in HPLC. Some of it is over my head but if there are questions I will ask him.

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showstoppa's picture

Why would anyone believe anything alin says? He has motive to slander the test, he also has a history of doing this as he did it to william Llewellyn in 2009.

Just a little word to the wise, never trust anything a source tells you. Alin might be right in the end but don't ever trust anything he says.

ScorchedEarth's picture

just commenting so i get notifications of new comments. Bye Smile

CBBurrr's picture

Me too, interested to hear what Labrat has to say.
It's nice having one member who really understands this stuff

Trenabolic's picture

Why do you guys take these guys words as gospel? I mean I'm not the smartest tool in the shed but it's obvious to me this labrat guy isn't as smart as he tries to portray but hey that's just me what do I know.

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CBBurrr's picture

I found his comments to be pretty believable
Do you think he was lying about being an analytical chemist?,

CBBurrr's picture

I looked at his older posts, He claimed to be a chemist back in 2012, so it's not something he just came up with to help out angus.

Trenabolic's picture

It's the net bro, if I tell u I'm Phil Heath would you believe me? He may or may not be I'm just saying I ain't buying it lol

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dooduu2's picture

People need to learn their lessons. Everyone thought Muta was guru. Turns out to be a zit faced kid.... Fooling everyone. Brilliant

I just assume everyone is a fat tranny living in their parents basement.

dooduu2's picture

Expect the worst, hope for the best.

You'll never be disappointed.

CBBurrr's picture

Bro, Are you really Phil Heath!! Smile
This has turned into the eroids lab challenge, and I've gotta root for someone, so I'm rooting for Angus.
I hope the truth comes out, either way.

Trenabolic's picture

Lol

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ashop's picture

LABRAT is part of Angus team. ( He also made mistakes in his statements. I pointed them.) Those guys are copying from manuals parts of good theory then twist the things so you accept their testing. How can you be so naive ? Some guy with a new name that never posted before popped out here when Angus had problems and posted some text copied from manuals then started twisting things into Angus favour. He can do analyzes if you do not care if they are not real

ashop's picture

I think that your credibility here is under 0. I bet he is the guy who is doing analyzes for you. Same style, lots of pages from manuals then twisting the words. Analysts are not like this. Analysts are very exact and do not play with theories.

I see you are now giving us diagnosis like a shrink Smile Are you a doctor now ? besides analyst Biggrin Biggrin

dooduu2's picture

It's looks like Dr may be a student... Or maybe a doctor that thought he knew what he was doing. But I like I said before with out any checks and balances a lot of ppl look stupid now.

ashop's picture

Angus you are the master of making money from snake oil. It is a shame to post such erroneous documents here claiming to be written by your doctor

dooduu2's picture

I think we should be skeptical of everyone.. You know money moves mountains. I do have a lot of respect for you, you have put your self out there in a crazy way. And the little you make from these tests isn't worth any of it.

I have never used alins gear nor do I plan on it.

I just a wish we had 3 of you. To check each other.

ashop's picture

If you look carefully they already are 3 chemists who help each other ....

ashop's picture

hobby than anything else.

Are you serious ? Is not the lie that bothers me but the insult to my intelligence

ashop's picture

Here is a comment from a chemist about your documents posted here. Please remember you posted that those documents were written by your analyst to be presented in the class.

====

Comments made by a specialist on this document

  1. The analysis was done incorrectly. The linearity test must have been taken by the standard solution, of different concentrations.
  2. The line cannot be taken into consideration if the value of approximation is lower than 0,99. This value is not present in your Figure 2B.
  3. The sample must be injected and the concentration mathematically calculated, using the formula stated in the Figure 2B. It’s incorrect to build the linearity out of a mix of the sample and the standard, from the very beginning.
  4. The “purity” of standard is 96,8, when calculating the values from your Table 1 (an enormous error for a standard).

We have nothing against the use of mass spectrophotometria method for identification and dosage of substance, but this method should be used properly, and the values calculated correctly.

==================

Labrat's picture

Yes the reference standard must be used to plot the calibration, and at 3 points, a one point such as this assumes linearity, which is not always the case.. You get an s shaped curve.. you have a minimum and maximum detectable threshold and the (hopefully) straight line in between where the relationship is proportional to the concentration. You can't just assume linearity based on one point on a graph

ashop's picture

Your point of view is the same as our professor
As a conclusion documents presented here by Angus( claim to be written by a doctor ) are INCORRECT.

Labrat's picture

Alin..do you want me to send you a screen shot of the perkin elmer spectrum quant sofware we use to quantify with the ftir?..im actually using it right now...of course you said this isnt possible. You may want to try telling that to Perkin Elmer and their chemical engineers..You obviously dont know shit about chemistry..only what info you find online..and if you arent a chemist..it is confusing
I suggested FTIR as something a source could use to qc raws they buy .(to id)..it can also quantify though its not commonly used.
Im sure not all sources can pay 300 for HPLC, GC/MS or LC/MS and I suggested FTIR as an OPTION..because they can buy one and use it themselves
As I said I am not trying to sell anyone anything..nor offer testing services..my job is worth way too much to risk that.
By the way since you are overseas..
Look up "infrared spectrometric purity control of chemical substances using R",
Also call the university if duisburg-essen department of chemistry and tell them to stop using FTIR to quantify with..because you say its not possible.
Never try to argue a topic you dont know anything about with a person who does..and who does it for a living.
You just make yourself look ignorant.

ashop's picture

Also call the university if duisburg-essen department of chemistry and tell them to stop using FTIR to >quantify with..because you say its not possible.

I will tell professor to call and be sure he will call because he speak German and will be interesting for him. Do you have the name of the person who is doing this or you just throw here a german name to sound interesting ?

ashop's picture

I see Labrat ( Angus and his team ) is nervous Smile Why did you come here when Angus was in trouble ? To convince people with your theories ? To convince everyone you are a good guy and want to help ? Why are you fucking around here with methods that nobody recommend them ? Do you want to scam people now with FTIR since MS is proved scam ?

I do not know nothing about chemistry, I never said I know. I just said I take your texts ( Angus, Labrat and who is in your team ) and I give to a professor who is laughing in my face asking me where I found those crooks and why I discuss with such guys

Anyway here is professor answer regarding FTIR. He said since you weak students no matter you have google in the front of eyes it will not help you. He told me you guys are some monkeys who use machines, not analysts

RESPONSE FTIR

FTIR is mostly used for identification. The device calculates the % of coincidence with the library data. One may use this method for quantification, but again, the device has spectra for near, far and middle region. A part of spectra is not expressed and will give a large error. You can`t do the quantification for the full spectra so you?ll have to use a limited area. The question is what area are you going to use? You can?t avoid validation, if you want the result to be reliable.

Thus one must absolutely use standards for quantification and analyst should be a person with experience not a freshman student

Labrat's picture

Are you gonna be one of those idiots who will argue with me about the boiling point of water?? Do you think the earth is flat?. or do you have to consult your "expert"on that also. Be sure to do your homework before making statements that are just ignorant.... run along to the professor and ask him why everyone is lying to you.

Here is how GCMS analysis is a "proved Scam" and how steroids "aren't volatile".. your words..
This is in fact a published method used for GCMS.. I hope you realize that whether its gas (GC) or Liquid(LC).. those are just the separation apparatus.. in either ithe compound passes to a detector "mass spec" or other.. so when you say "since MS is proved scam ?" exactly what do you mean??
LC is advantageous because there is no dervitisation required. so sample prep is minimal.. however there are some steroids that can't be analyzed with LC , but can be with GC, it is dependent upon the saturation of the molecule..
why would you think Agilent sells GC columns specialized for steroid analysis?? You think they sell these columns for GC, yet according to you .. its just not possible right? I wonder why they manufacture these columns if its impossible to use them for their intended purpose.... do yourself a favor quit thinking there is a conspiracy against you..why dont you research this for yourself?
and stop making dumbass statements when you have absolutely no clue what you are talking about.

GC-MS analysis was carried out using an Agilent 6890 Plus gas chromatograph interfaced with a single-quadrupole Agilent 5975 MSD. The electron energy was 70 eV and the ion source temperature was 230°C. Each sample (2 μL) was injected in split mode (10:1) at an injector temperature of 280°C and was separated through an Ultra-1 capillary column (25 m × 0.2 mm i.d., 0.33 μm, film thickness; Agilent Technologies). The oven temperature was initially 215°C, which was ramped to 260°C at 1°C/min and then finally increased to 320°C (hold for 1 min) using a 15°C/min ramping program. Ultrahigh purity helium was used as the carrier gas with a column head pressure of 210.3 kPa (column flow, 1.0 mL/min at an oven temperature of 215°C). For quantitative analysis, the characteristic ions of each steroid were determined as their trimethylsilyl (TMS) derivatives. Peak identification was achieved by comparing the retention times and by matching the peak height ratios of the characteristic ions

So there you have a standard procedure for qualitative AND quantitative analysis using GC/MS.
which isnt even possible right?? Looks like they somehow got steroids Which"aren't volatile" to phase change to gas at 320C these guys are violating YOUR physical chemistry laws???? must be a conspiracy..

Google GCMS analysis of steroids.. or GC retention indeces of steroids and see if you can figure out why the entire scientific community, save for one profesor , has ganged up against you..

ashop's picture

Someone said here ( Nitti if I remember): If you can not explain in a simple way even you do not understand it. Or I can add maybe you just wanna confuse us Smile

Trenabolic's picture

CALL SOMEONE ELSE AN IDOT AGAIN AND I WILL MAKE YOU LOOK LIKE AN IDIOT BY GIVING U A TROLL TAG, IS THIS CLEAR ENOUGH FOR YOU?

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ashop's picture

You are funny

About using the gas chromatography for quantification

Surely it is used for volatiles, but only if the melting and vapor temperature are lower than the decomposition temperature

If the substance melts while decomposing, we will find results of decomposition, whether we use mass of chromatography. For example - Testosterone Cypionate is quantified with USP on gas chromatograph but in your ( Labrat ) example was testosterone enanthate product that goes into decomposition at 40 C. So you Labrat, you just read something somewhere but you are not understanding. You are educated in this matters but you are not a analyst. Maybe in 5 years but thats my opinion sure

this comment was not made under professor advice but I think is right, I will have his comments also

https://en.wikipedia.org/wiki/Gas_chromatography

Gas chromatography (GC), is a common type of chromatography used in analytical chemistry for separating and analyzing compounds that can be vaporized without decomposition

Testosterone enanthate goes into decomposition at 40 C,

Here is your post where you were giving me lessons how to use a GC on testosterone enanthate. Maybe you feel some shame now ?

Now you are just being ignorant. Not volatile?..lol...okay at 760m Hg testosterone enanthate boils at >432.9 degrees celcius. Thats at atmospheric pressure. The gcms is operating at close to a >vacuum..And in a vacuum the bp drops (educate yourself)more so with a turbo pump.,than with a >diffusion pump. If you are trying to say that steroids arent volatile..then you are saying that the steroid >would never go from liquid to gas, and never elute from the column to the MS. That means every gcms >spectra that anyone can view at thousands of websites is all just a lie.
Listen, I don't know Angus from Adam. I agreed that from what I saw the results were questionable and >could be innacurate..I completely agree with you there The preferred method for quantifying? HPLC.. >or LC/MS...?..definitely ..no dispute Can you quantify with GC/MS. ?..yes and very accurately with >reference standards..
Can you quantify without standards?..yes but you would have to know exactly what the impurites are.. >would this hold up in court?..no I work with 6 different GC/MS..an ICP/MS. 2 HPLC, 2 LC/MS , FTIR >UV-VIs, the only thing we dont have is an NMR We get unknowns all the time and we must Id and >quantify..
I wish you the best of luck..I was only offering information about what we do in a real analytical >lab...believe me, if I didnt know what I was doing I wouldnt have a job..and Ive been doing this for a long time.

Labrat's picture

Spectroscopy
Volume 26 (2011), Issue 2, Pages 93-104
http://dx.doi.org/10.3233/SPE-2011-0529
Quantification of carbohydrates in fruit juices using FTIR spectroscopy and multivariate analysis

There alin..here is good example of how you CANT QUANTIFY with FTIR?..Right that was what you and your professor said?..
What school.did this 'professor" go to?..
ANY analytical chem..even student would know that you can
Its not commonly used but it can be accurate to about 3 to 5%
Gcms?..1%
GC with FID detector?..0.1%..

Again its insulting for you to tell me its impossible to quantify with FTIR and im actually at work..using FTIR to quantify with. Thats not stupid..just ignorant..go take a few years of chemistry and then perhaps we can have a productive conversation

ashop's picture

This discusion may never come to an end. Nobody says that one can’t do quantification using HPLC, GC, FTIR, MS…The only thing we disagree with is the way you do the analysis, its reliability and the interpretation of the obtained results. It was an incredible pleasure for us to read the article about the carbohydrates dosage in different kind of juices.
The stages of analysis are clearly stated:
a) Obtaining the standard (using HPLC, in this case HPLC uses an CRS for different carbohydrates).
b) Comparing the juice samples with the standards obtained with FTIR.
c) The complex processing of the obtained data.
Let’s insert a dose of humor to our discussion: We talk about juice right now. The measurement unit for carbohydrates is gr/100 ml. What are the consequences of a 50 % error? 0%! +- 1-2 gr of fructose per 100 ml of juice. But back to science! The scientific literature has articles about dosage methods of medicaments using FTIR. They may be found all over internet. They’re about a clear staging of analysis, followed by processing the obtained data.

It’s now very clear that Labrat etc tries his best to make Angus look reliable. They speak about both traditional and new literature methods of analysis, claiming we do not accept them, but they never speak about where and how these methods are used by Angus. You can’t do an analysis by making two injections in mass, GC, FTIR… and comparing them with Hell knows what. Let’s be scientifically correct and stop protecting some internet con artists, which aren’t even analysts.

ashop's picture

This study was done by 3 romanian universities. Be sure that I will get informations for you regarding their error and I will get back to you.

But IMO you just run a search on google and found that title. Is one thing to do the quantification of the carbohydrates in fruit juices and one thing to do the quantification of drugs. Who needs exactitude for fruit juices carbohydrates ? But thats my opinion.

I will not any year in chemistry my friend I am not making money selling fake MS here on the board. Now you guys see that MS are proved unreliable and you come with another method nobody heard.

Labrat's picture

An option.. good one actually... do whatever you think works best for you okay..I am not suggesting to anyone to use FTIR to quantify with.. its certainly not the best way.but you CAN thats the point. and you could take samples that you have validated.(GCMS/HPLC.. whatever). run these on the ftir, save the spectral image. and compare future samples to them.. it would save you a lot of time and money.. and be very effective..

ashop's picture

I have the proves that Angus is doing shit and now I do not trust anyone. Call me stupid or whatever. Please stand back lets him stand for his money who took and all the shit he had done then my friend you get from me anything. Lets not make this thread another war thread. Lets post only to subject i

Labrat's picture

I used FTIR as an option that someone with no experience can use . FTIR CAN be used to quantify. I use a perkin elmer spectrum 2 and it has quant software. We use it ti quantify with on occasion
The proper method is definitely LC/MS , GCMS, HPLC MS
What you can do..is once you have verified purity %..you can scan these on ftir..okay?..then FUTURE batches of raws can be scanned and compared..if it fails FTIR..you have a problem .
in fact one of out primary uses of ftir is qc of raw materials..if it fails FTIR..we reject it..no need to test further with GCMS HPLC, etc..
I honestly dont know Angus.. I answered questions based on experience and knowledge. with no bias or alterior motive. If you remember I told you that reference standards are required..and minimum 3 point calibration plot to be accurate. Otherwise it is just an estimation..Thats a given..But again..how accurate do you need to be?.
If it were me..I would have raws purity verified HPLC..I would then scan these on FTIR..I would build an FTIR reference library..Then when I got new raws I would scan and compare to the known pure reference FTIR library...It would save a lot of money..and like I said ..you can buy one relatively inexpensively . OR you can pay 300 to 500/ test for every lot of every batch of raws you get..and HOPE that you are getting the right results. ..Do what you want..Do I care?..No. Best of luck

ashop's picture

definitely LC/MS , GCMS, HPLC MS

If you say that the proper method is definitely LC/MS , GCMS, HPLC MS, why you come here now when we are questioning MS methods ( even you see this article posted by Angus in this thread is a error ) and confuse people and me also? Just wait until the smoke clears then you are welcome to show your view. Even HPLC is not good if the analyst is bad. Why otherwise professor would not let students to make analyses for me after-hours so he can cover a larger volume ?

My friend LABRAT, I do not trust you from few obvious reasons. First because you a just hibernated all this time when Angus was scamming people here and poped out when Angus was under pressure. Second because you promote undocumented methods based on your word.Now you come here same style as Angus TO HELP and sure some of the explanations you give are partially correct but also can copied from manuals or just explained in a wrong way by a guy who is not able to understand for himself. I suggest you if you want to prove you honest to wait until Angus is proved wrong or right then you can pop out again to offer your services or your help. Stand back till Angus is clearing his shit then I will treat you with respect. I dont not trust anyone now since I saw what twists Angus can do

ashop's picture

be Careful of the snake oil.

please come with arguments do not do again WOB

I have so much to do today I cannot play your games sorry.

Angus those are not games. I do not play with my reputation and I do not play with anything.

Anyway you said you are a middleman and not the analyst. Send my chemist answer to your doctor then post his answer exactly on each point. Then I take your answer and I send to my professor.
We are just middleman and we post here conversations between two chemists. Then members of this board will learn and decide with their own brain who is right or not.

Lets not do WOB ( waste of bandwidth ) until the original message is lost like you have done with other threads. You still have lots of explanations to give. Please do not post again meaningless messages until you have arguments to the letter my professor wrote

ashop's picture

People in Moldova work a lot. Do you need this email or you have already ? Discuss directly with him
Again you bring in discussion anything just no arguments. Thats not very responsible for a analyst who made some good money from testing. ( thousands of analyses like you told me )

Plus minus 10% concentration is poor quality. What you mean about purity is about API my man.
In final product we discuss about concentration and presence of impurities according to pharmacopeeia , please I gave you a lot of documents already. Even I started to know some terms. Please try to speak analytical correctly.

I see you try very hard but there is no perfect crime there is no perfect lie. Remember this !

Third party lab, certified lab that is testing according to pharmacopeeia. If you want to test we should do a cross check just to avoid fraud. In rest I am ready to pay.

ashop's picture

I don't ask anyone to trust me, lets say how some said because I sell products
I think also you should not trust Angus because he also sells his services. He doesn't do a free service to community.
Plus in all Angus analyses and post he made until this moment there are many wrong things I have pointed ( I will make a summary to everything later ) but anyway he avoid to answer to those parts in my posts, he just picks up irrelevant parts of my comments and answer to those ones.

JUST READ AND THINK WITH YOUR OWN BRAIN. TRUST LOGIC AND MATHEMATIC.