Testing Protocols

[rmtt]

This has always interested me. I've worked in chemicals my entire career. Although I'm an electrical engineer.....I have access to a lot of testing equipment...(HPLC, GC,etc).

A colleague of mine is over all the labs in our facilities......and I've known him forever. Though I would never approach him about this type of specific testing....is it basically the same as anything else?

For example...when we get in a raw material....we already have a "control standard" in our HPLC database.

We then run the raw...and compare the peaks. This shows us purity levels, and also minor impurities if we see other "spikes" on the graph even if they are very small. I'm talking like PPM (parts per million).

We can even identify the impurities as we have a very large database of compounds logged to compare against.

Just wondered if it was as simple as that.

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[rmtt]

Another thing is that we can also test finished goods. These can contain multiple compounds....but we can see exactly what is in each sample....and percentages of different compounds in relation to the others.

Its always fascinated me. I may have to spend a little more time around the lab then I normally do.

Since I'm the plant engineer....I'm responsible for all process automation. These tests are some of the things I use for troubleshooting potential issues when a reaction doesn't go as planned...or if QC is slightly out of kilter.

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[buck1973]

I will Blow a message into Our lab and have this answered.
it sounds very similar to how the process we use works..
there is a European Pharmacopoeia (EP) Reference Standard that is tested and calibrated before our sample.
there is a graph with peaks and valleys at different lengths
this is the raw data , dependin were these peaks come in is the compound and quantity...
blends are identified by multiple peaks and amounts

 

[rmtt]

I will Blow a message into Our lab and have this answered.
it sounds very similar to how the process we use works..
there is a European Pharmacopoeia (EP) Reference Standard that is tested and calibrated before our sample.
there is a graph with peaks and valleys at different lengths
this is the raw data , dependin were these peaks come in is the compound and quantity...
blends are identified by multiple peaks and amounts

No worries.....just thinking out loud. Also just a note to people that may read this...

This type of equipment is very expensive....it would blow your mind how much our equipment cost....plus the annual costs to keep it calibrated.

To have access to this type of testing for the meager amount of money we are donating......you can't emphasize enough how valuable this is.

A lot of places can't afford this equipment....and we actually test products for a lot of companies in our area even though it's not part of our business model.

It's hard to find....and even harder to make arrangements considering the compounds that we are testing considering they are illegal in most places.

I actually plan to make another donation once I get this semester behind me...(daughter is in her first year of Med School).

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[buck1973]

No worries.....just thinking out loud. Also just a note to people that may read this...

This type of equipment is very expensive....it would blow your mind how much our equipment cost....plus the annual costs to keep it calibrated.

To have access to this type of testing for the meager amount of money we are donating......you can't emphasize enough how valuable this is.

A lot of places can't afford this equipment....and we actually test products for a lot of companies in our area even though it's not part of our business model.

It's hard to find....and even harder to make arrangements considering the compounds that we are testing considering they are illegal in most places.

I actually plan to make another donation once I get this semester behind me...(daughter is in her first year of Med School).

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Jano And myself had this very convo as far as new machines aval. and he is constantly upgradin or replacing equip. i have vids of this equip in use that i thought was intrestin but its very sensitive so it cannot b posted...

 

[rmtt]

Jano And myself had this very convo as far as new machines aval. and he is constantly upgradin or replacing equip. i have vids of this equip in use that i thought was intrestin but its very sensitive so it cannot b posted...

Completely understand. When we test for other companies....we actually make them sign a NonDisclosure agreement.

Also just having the equipment means nothing. You need to have a qualified technician to ensure proper Standard Operating Procedures.

Without that.....too many variables that could affect things. But once properly setup....these things are very precise. Resolution is amazing.

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[AnaSCI]

This should make for a good discussion.

Would like to hear jano's input or also any others in the field.

Thanks rmtt!

 

[janoshik]

I am in the lab right now, dealing with insane number of samples but I should be done in 24-48 hours and I'll get onto this! (if I don't, please, remind me )

Surely will lead to an interesting discussion.

 

[janoshik]

So, I've finally found time for this.

From what you are saying I assume that you are using HPLC coupled with mass spectrometer (I assume so from "'control standard" in our HPLC database" which imo implies for mass spectra).

With mass spectrometer as the detector it is MUCH easier to identify compounds or impurities.

However, there is a trade off - keeping mass spectrometer stable and working costs incredibly much and requires a lot of additional tech.

I've played around with the thought, but instead I've chosen a different detector - UV/VIS and ELSD.

With those, esp. UV/VIS the identification is not as straightforward and requires more care from the operator, but is literally maintenance free and QC can easily be automatized.


It might be important to point out, that the percentages you get from the mass spectrometer (like peak 1 is 80%, peak 2 20%) are not always real. It depends a lot on the properties of the compound - for example some are not easily ionized and it's possible that the 20% peak is in reality 98%.

This is the reason why standards are necessary most of the time.

(In relation to this, topic of universality of response of ELSD might be an interesting read. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3338159/ )

 

[janoshik]

No worries.....just thinking out loud. Also just a note to people that may read this...

This type of equipment is very expensive....it would blow your mind how much our equipment cost....plus the annual costs to keep it calibrated.

To have access to this type of testing for the meager amount of money we are donating......you can't emphasize enough how valuable this is.

A lot of places can't afford this equipment....and we actually test products for a lot of companies in our area even though it's not part of our business model.

It's hard to find....and even harder to make arrangements considering the compounds that we are testing considering they are illegal in most places.

I actually plan to make another donation once I get this semester behind me...(daughter is in her first year of Med School).

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It's absurdly expensive, true, but with right choices the costs can be decreased a lot.

A lot of the most expensive stuff is for convenience, so I often rather spend more time doing work manually than investing in the most expensive stuff.


I'm using Shimadzu Prominence UFLC and Shimadzu Nexera-i LC-2040C 3D (and Shimadzu ELSD-LTII) for my work and it's sufficient for now.

And thanks god working with limited amounts of anabolics is not illegal where my lab is based at


Wishing the best of luck and lot of patience to your daughter, been to med school myself!

 

[rmtt]

Yeah...we have a HPLC coupled with mass spectrometer.

In fact...we just ordered another one today as the manufacturer is offering "special" pricing. Still set us back around $80K.

We have UV/VIS equipment as well.

Some of our customers want detailed reports....others just general QC data.

We deal with some pretty nasty stuff.....we have every state and federal agency routinely inspect our facility....including Department of Homeland Security.

But we run a tight ship.....and we get bloodwork and physicals on a regular basis which I'm able to use for my own benefit to keep tabs on how certain things affect me!

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[rmtt]

So, I've finally found time for this.

From what you are saying I assume that you are using HPLC coupled with mass spectrometer (I assume so from "'control standard" in our HPLC database" which imo implies for mass spectra).

With mass spectrometer as the detector it is MUCH easier to identify compounds or impurities.

However, there is a trade off - keeping mass spectrometer stable and working costs incredibly much and requires a lot of additional tech.

I've played around with the thought, but instead I've chosen a different detector - UV/VIS and ELSD.

With those, esp. UV/VIS the identification is not as straightforward and requires more care from the operator, but is literally maintenance free and QC can easily be automatized.


It might be important to point out, that the percentages you get from the mass spectrometer (like peak 1 is 80%, peak 2 20%) are not always real. It depends a lot on the properties of the compound - for example some are not easily ionized and it's possible that the 20% peak is in reality 98%.

This is the reason why standards are necessary most of the time.

(In relation to this, topic of universality of response of ELSD might be an interesting read. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3338159/ )

Very true. Most of the companies we deal with wanting that detail are getting products that are supposed to have only one peak. Anything else that shows up is usually a problem for them. But again we are looking in the PPM range.

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[janoshik]

Very true. Most of the companies we deal with wanting that detail are getting products that are supposed to have only one peak. Anything else that shows up is usually a problem for them. But again we are looking in the PPM range.

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Same when I am testing raws, yeah.

On the topic of government control I just have all my packages opened and tested if they comply with the regulations. That's been enough so far.