T-Bagger
Elite
Name and shame bro!
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Anabolic Steroids
Janoshik Analytical laboratory testing services
- Thread starter janoshik
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janoshik
Subscriber
I have stated it in public on BOP before, that it is certain that there was no mistake made when the samples were tested after which there were 2 sources banned on BOP. One of them along with their rep is spreading easily verifiable lies about me as we speak. All I'm going to say.
Good night.
Klimmzugernie
Well-known Member
@janoshik you could immediately stop this discussion by posting a picture of your equipment. Why you don't do that?
janoshik
Subscriber
But I already did and there is no discussion - Janoshik Analytical laboratory testing services
You can't expect me to waste my time by reacting to self admittedly mentally ill person, such as master.on.
Klimmzugernie
Well-known Member
Doug_S
Member
Jano,
Just put or curiosity, what is your QA/QC, Data Quality Objectives, and validate processes in general?
I review a ton of data and we require Level IV data, which means we do not consider data validated until we get a full instrumentation package from the lab.
I see shitty things some analysts do like run their performance blanks first thing is the AM when the lab is quiet and clean instead of Midway through their runs like they should. I deal with volatiles a lot so that pisses me off.
Sometimes I see a lot of contaminants in a sample like acetone or methonal show up on a lot of samples = dirty lab or sloppy extraction technique.
I see labs do lazy shit. They usually dilute every sample in case we get a real hot one so it won't blow their columns and leave artifacts for a month. Then instead of re-running, they will simply j-flag the shit with too high of a Detection Limit and corresponding LOD for me to use.
What does validation look like with these chemicals?
janoshik
Subscriber
Now in English please
You know I ain't expert on that - any advice and suggestions will be welcome.
Methods were validated at 3-5 calibration points, all good linear with big enough range, most of the samples are within 2 orders of magnitude anyway... LOQ and LOD are not really an issue with this kind of work either. Specificity is not an issue either, as we are not expecting huge interferences from something in concentration as high as AAS would be, UV spectrum + retention time work well so far, except for awful compounds such as drostanolone, which have extremely low UV absorbance and can be hidden by interferences. Spectral deconvolution sometimes work, other times I gotta use column with different selectivity.
Standards are external, sometimes ran at the end of the analyses of the unknowns, sometimes bracketed. I have to admit I do brackets only when I have unusually low workload, as there had never been any real difference in the resulting data. CCs are nice and linear in the working region so after they were established only 1 point CC is used most of the time.
It's not like I deal with trace samples, volatiles or difficult matrix. There is no extraction going on - I live by the rhetoric that less is more with sample prep. Less I do the less there is to fuck up.
Oil samples are diluted in methylene chloride or chloroform 100x and injected in sub 1 ul amounts - usually 0.5ul, which had been found to work great precision and solvent effects-wise.
No real extraction issues, no contamination issues as 10 ul pipette tips are single use and so are the autosampler vials.
Pill samples are sonicated in solvent, usually methylene chloride then filtered to sample vial. Again, all that comes into the contact with the sample is single use. There are no real losses with MC due to evaporation, as the time in the open is usually less than second or two. Autosampler is cooled and that keeps the precision great for longer than necessary, even after the seal on the autosampler vial is broken by sampling needle.
Peptides and GH are dissolved in 2 ml water and shot as it is.
I tried to minimize the potential places for issues, but still, something stupid always happens.
---
After the system is warmed up, blank is shot in twice or thrice to get a clear baseline.
System suitability is run at the start of the day and at the end:
1ul injection of cca 0.5 mg/ml testosterone decanoate, testosterone enanthate and testosterone cypionate* (or another critical pair)
Retention time of testosterone decanoate ( PASS: < 0.02 min SD from previous measurements )
Area of testosterone decanoate ( PASS: < 1% SD from previous measurements )
Resolution between testosterone enanthate and cypionate ( PASS: > 1.5 separation to valley )
3x injection of caffeine 0.1-2 mg/ml
Retention time of caffeine ( PASS: < 0.02 min SD from previous measurements )
Area of cafferine ( PASS: < 1% SD from previous measurements )
UV spectrum of caffeine ( PASS: UV lambda max and UV lambda min within one or two nm of their theoretical values)
RSD of caffeine ( RSD < 0.3% for the 3 injections )
1x Blank after caffeine injection ( PASS: caffeine carryover under 0.01% at caffeine lambda max )
System hardware check is run once per two weeks.
This takes care of the most system related variables and if there is a problem, I catch it even before I start working.
I throw in a well characterized sample which was prepared along with the batch of the samples that I'm dealing with here and there. Just in case something was wrong with the solvent, pipette, sonicator etc.
Now in English please
You know I ain't expert on that - any advice and suggestions will be welcome.
Methods were validated at 3-5 calibration points, all good linear with big enough range, most of the samples are within 2 orders of magnitude anyway... LOQ and LOD are not really an issue with this kind of work either. Specificity is not an issue either, as we are not expecting huge interferences from something in concentration as high as AAS would be, UV spectrum + retention time work well so far, except for awful compounds such as drostanolone, which have extremely low UV absorbance and can be hidden by interferences. Spectral deconvolution sometimes work, other times I gotta use column with different selectivity.
Standards are external, sometimes ran at the end of the analyses of the unknowns, sometimes bracketed. I have to admit I do brackets only when I have unusually low workload, as there had never been any real difference in the resulting data. CCs are nice and linear in the working region so after they were established only 1 point CC is used most of the time.
It's not like I deal with trace samples, volatiles or difficult matrix. There is no extraction going on - I live by the rhetoric that less is more with sample prep. Less I do the less there is to fuck up.
Oil samples are diluted in methylene chloride or chloroform 100x and injected in sub 1 ul amounts - usually 0.5ul, which had been found to work great precision and solvent effects-wise.
No real extraction issues, no contamination issues as 10 ul pipette tips are single use and so are the autosampler vials.
Pill samples are sonicated in solvent, usually methylene chloride then filtered to sample vial. Again, all that comes into the contact with the sample is single use. There are no real losses with MC due to evaporation, as the time in the open is usually less than second or two. Autosampler is cooled and that keeps the precision great for longer than necessary, even after the seal on the autosampler vial is broken by sampling needle.
Peptides and GH are dissolved in 2 ml water and shot as it is.
I tried to minimize the potential places for issues, but still, something stupid always happens.
---
After the system is warmed up, blank is shot in twice or thrice to get a clear baseline.
System suitability is run at the start of the day and at the end:
1ul injection of cca 0.5 mg/ml testosterone decanoate, testosterone enanthate and testosterone cypionate* (or another critical pair)
Retention time of testosterone decanoate ( PASS: < 0.02 min SD from previous measurements )
Area of testosterone decanoate ( PASS: < 1% SD from previous measurements )
Resolution between testosterone enanthate and cypionate ( PASS: > 1.5 separation to valley )
3x injection of caffeine 0.1-2 mg/ml
Retention time of caffeine ( PASS: < 0.02 min SD from previous measurements )
Area of cafferine ( PASS: < 1% SD from previous measurements )
UV spectrum of caffeine ( PASS: UV lambda max and UV lambda min within one or two nm of their theoretical values)
RSD of caffeine ( RSD < 0.3% for the 3 injections )
1x Blank after caffeine injection ( PASS: caffeine carryover under 0.01% at caffeine lambda max )
System hardware check is run once per two weeks.
This takes care of the most system related variables and if there is a problem, I catch it even before I start working.
I throw in a well characterized sample which was prepared along with the batch of the samples that I'm dealing with here and there. Just in case something was wrong with the solvent, pipette, sonicator etc.
Cool. Hey can you post up some of that data. Specifically, let’s have a look at the Bold cyp/Deca analysis that everyone is currently buzzing about. Your reports just give results but let’s have a look at the printouts.
I can get you a copy of the posted results if you need me to go get it for you. But I think you already know which one I’m talking about.
janoshik
Subscriber
Sure, give me a minute.
janoshik
Subscriber
The Nandrolone Decanoate peak is fairly obvious in there.
The UV spectrum fits deca as well.
The UV spectrum fits deca as well.
janoshik
Subscriber
@BigBaldBeardGuy Any questions you got, shoot. Any discrepancies you find, shoot.
Thanks Jano.
What’s the concentration of BB and can you confirm no BA?
What’s the concentration of BB and can you confirm no BA?
janoshik
Subscriber
I honestly have no idea, I don't measure it.
I could measure it by shooting up some BB standard and comparing it to old data, or shoot the sample again - I keep samples for 14 days usually.
Or it could be measured, if we trust TGI, by asking him what % BB he puts there and by comparing it.
Regarding BA, you won't see it on the sheet I exported - it's at 240 nm and BA doesn't absorb (can't be seen) at that wavelength.
janoshik
Subscriber
However, when I take a look at lower wavelengths, something I would judge to be benzyl alcohol can be seen in substantial enough concentration.
(In red circle )
(In red circle )
It’s not TGI. Other lab. But I think it might be useful for you to get the BB concentration. If people think the sample was tampered with by the member that submitted it then the BB concentration might also be different.
Edit: don’t post that BB concentration in the open. Hold onto it.
janoshik
Subscriber
Now, if you notice that there is a straight line right under the peak in red circle - which is what I (based on experience) judge to be benzyl alcohol. That straight line shows which peak has its UV spectrum shown in the upper right corner of the image.
You can see there the UV spectrum of the said peak. Now my experience would not be a good enough evidence for many over here, so we can use that.
After you google "benzyl alcohol UV spectrum," this is one of the links that pop out:
Oxidation of aliphatic alcohols and benzyl alcohol by H2O2 under the hydrothermal conditions in the presence of solid-state catalysts using batch and flow reactors - PDF Free Download
You want to check page 4 (Fig. 3) and you can see that there is spectrum for BA. If you look very close, you can see that the tiny peak at 257 nm is there as well, so we can conclude that in the sample tested there was BA, based upon objective evidence.
You can see there the UV spectrum of the said peak. Now my experience would not be a good enough evidence for many over here, so we can use that.
After you google "benzyl alcohol UV spectrum," this is one of the links that pop out:
Oxidation of aliphatic alcohols and benzyl alcohol by H2O2 under the hydrothermal conditions in the presence of solid-state catalysts using batch and flow reactors - PDF Free Download
You want to check page 4 (Fig. 3) and you can see that there is spectrum for BA. If you look very close, you can see that the tiny peak at 257 nm is there as well, so we can conclude that in the sample tested there was BA, based upon objective evidence.
janoshik
Subscriber
I know this is sample of Pristine lab.
I meant I can't really test BB right now, I'm thousand kilometers from the lab. However, I can compare the data from the TGI's samples, which have been tested around the same time, to this sample to get some answer. Considering all TGI's samples have been immaculate I figure he knows what % BB he puts in his oils, so that can be used as a very crude reference sample.
I'm sorry if I'm not being clear, just sharing my line of thoughts.
I understand your thinking there but in this case because so many people are looking at it I think it would be better if you pulled the result yourself when you get back to your lab. Whichever way makes you more comfortable defending it.
janoshik
Subscriber
I'm quite impatient, I asked TGI and I'll be waiting for his reply.
It's quite exciting, to be honest. I've attached the raw data to TGI's mast p, so all the data are as transparent as it gets.
No mistakes or no excuses. If that means doing the analysis again to make it defensible and clear then that would be the best to do.
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