Standards Used in Testing

[highonmt]

I used HP because it was suggested to me by researchers I knew.
It also allowed simultaneous two injection ports with different columns to allow separation of CBD from CBC, that and an autosampler tray for samples to be injected that holds 96 samples, to be run over night.
Compatible with GC/MS and a head space auto sampler.
And HP service.
-SamS

Sounds like a good setup. Do you own the auto sampler and dual columns...if so a very nice set up indeed with great throughput. The perfection of the autosampler was a real blessing to us chemists. That and the autoshimming feature on the nmr were the too biggest time savers in my short 25 year history. Oh and that last sentence is priceless when you are trying to get things done and a qhost pops up in your machine it makes that purchase price seem really reasonable... HP has good support personal ime better than those english as a second language flunkies populating some companies help desks.HM

 

[highonmt]

Thanks for the input brother Sam! I like HP equipment too and am in fact typing this on one!

Alas, I'm also on retirement income these days too and so always looking for "such a deal". Local testing gets prohibitive fast, and it doesn't take long to amortize out the cost of our own machine, so I've been trolling for a good deal.

Since broaching the question, I seemingly successfully bid on a used Perkin Elmer 8500, ostensibly fully operational with software and manual.

Any of ya'll have any experience with one of them?

Yep We had a couple of them in our organic chem lab. Nice simple set up youre glad it comes with a manual tho the software is old school...as I remember goto f1 is the 'abort' button. There is a whole table of shortcuts in the manual what detector did it come with.

 

[eloquentsoution]

we are privileged to have your professional input, HOM. thank you.

 

[Gray Wolf]

Yep We had a couple of them in our organic chem lab. Nice simple set up youre glad it comes with a manual tho the software is old school...as I remember goto f1 is the 'abort' button. There is a whole table of shortcuts in the manual what detector did it come with.

Thanks bro!

Not sure what all is in the packge yet, but the inventory sheets and paperwork should be arriving shortly and more will be revealed.

I bought it from a reputable dealer as a working unit with extras, which was operating when it was replaced by a new unit. I'm hoping it is good enough for our internal research purposes and parts and accessories appear to be still readily available.

Given the number of analysis we require for research, at about $100 per test with discount, having an outside lab do our testing is a deal breaker.

 

[Macola]

Gray Wolf, can you share the dealers contact and price ? Via PM, if this is too public.

 

[highonmt]

Thanks bro!

Not sure what all is in the packge yet, but the inventory sheets and paperwork should be arriving shortly and more will be revealed.

I bought it from a reputable dealer as a working unit with extras, which was operating when it was replaced by a new unit. I'm hoping it is good enough for our internal research purposes and parts and accessories appear to be still readily available.

Given the number of analysis we require for research, at about $100 per test with discount, having an outside lab do our testing is a deal breaker.

It should work great for the semi-quantitative analysis of most thermally stable compounds. Does it have an fid[flame inonization] dectector or tcd [thermal condutivity] these two dectors are the most common the fid will work great for cannabinoid analysis. I you want to do purity testign npd [nitrogen phosphorous] dectors are great if you are looking for pesticide residues. With this two column set up you can use a double ferrule to split your injections half to one column with a npd one with fid/tcd. Post up if you are having problems or just pm me. HM

 

[KiefSweat]

Given the number of analysis we require for research, at about $100 per test with discount, having an outside lab do our testing is a deal breaker.

that price should drop.

package deals are about 1/4 of that price here now and single tests half that.

 

[mofeta]

Here is another "materials and methods" quote for chemical investigation, by both GC and HPLC

Phytochemistry methods
Approximately 2 g of the dried plant material was extracted with
200 ml methanol:chloroform (9:1 v/v) by sonication at room
temperature (21
C), the standard extractive technique for this
laboratory (GW Pharmaceuticals), a method that recruits >95% of
phytocannabinoid content. The solvent layer was then transferred
through a paper filter into a rotary evaporator flask. The flask was
evaporated to dryness at 40
C, under reduced pressure, prior to
resuspension in 4 ml of methanol:dichloromethane (3:1 v/v). This
sample was transferred to two autosampler vials to be analysed by
GC-FID-MS and HPLC-UV. At all stages, the clean glassware was
extracted with the same solvents to ensure that none of the observed
peaks would be a result of contamination. GC-FID-MS analyses
were performed on a HP6890 gas chromatograph, coupled to a 5975
inert mass spectrometer. The system was controlled with Agilent
MSD chemstation D.03.00.611. The GC was fitted with a Zebron
fused silica capillary column (30 m30.32 mm inner diameter)
coated with ZB-5 at a film thickness of 0.25 lm (Phenomenex). The
oven temperature was programmed from 70
C to 305
C at a rate of
5
C min
1. The injector port and the transfer line were maintained
at 275
C and 300
C, respectively. Helium was used as the carrier
gas at a pressure of 55 kPa. The injection split ratio was 5:1. HPLC
profiles were obtained using an Agilent 1100 series HPLC system
controlled by Chemstation version A09.03 software. Cannabinoid
profiles were generated using a C18 (15034.6 mm, 5 lm) analytical
column fitted with a C18 (1034.6 mm, 5 lm) guard column. The
mobile phase consisted of acetonitrile, 0.25% w/v acetic acid and
methanol at a flow rate of 1.0 ml min
1 and the column was kept at
35
C. The UV profiles were recorded at 220 nm.

This is from that Russo paper about the 2700 year old weed they found in China. For those of you who haven't read it, here is a link:

Phytochemical and genetic analyses of ancient cannabis from Central Asia

It is definitely worth a read. The pot was found in the tomb of a guy who was part of a tribe of white people that lived in China ~3000 years ago. The area they lived in is a desert, and the weed was so well preserved that it looked like you could still smoke it! It had seeds that looked sproutable too.

They found like a pound and a half of it, someone had to have smoked some (I hope), I wonder what it was like.

 

[Sam_Skunkman]

No.

-SamS

Since broaching the question, I seemingly successfully bid on a used Perkin Elmer 8500, ostensibly fully operational with software and manual.

Any of ya'll have any experience with one of them?

 

[zeppelindood]

Great thread Kief... thank you for an awaking on the subject ya'll... specifically Sam and High

 

[Gray Wolf]

Gray Wolf, can you share the dealers contact and price ? Via PM, if this is too public.

http://myworld.ebay.com/capital-equipment

 

[highonmt]

Here is a paper in which gc data and gc-ms data are compiled the lists of retention times could be useful to someone doing analysis of cannabis. http://cpb.pharm.or.jp/cpb/201002/c02_0201.pdf

 

[Green Supreme]

Lots of good info folks. Thanks for sharing. Peace GS

 

[elmanito]

Essential oil of Cannabis is already for many years produced in Switzerland.Actually i'm glad that more companies are analysing or is interested in the terpene fraction of Cannabis.Essential oil has great medicinal properties.Use essential oils for years.

Company i'm talking about

http://www.olison.ch/4598.html

Namaste

 

[KiefSweat]

In order to obtain 1 litre of essential oil, we have to distil about 650kg of hemp (=1.5 litres for a ton of green hemp)

wow

 

[GrassMan]

Hi,
I’m not an analytical chemist but we’ll be working with a lab that will make us some cannabinoid analysis. Basically we’ll analyses the following cannabinoids. Each cannabinoid or molecule has a CAS number which indentifyes univoquely. Most of our desired cannabinoid to be tested will be supplied by Sigma Labs (which I’ve been told that are good quality) prior Government license (Israel).
Each test is done 3 times to confirm results.
The laboratories operate in accordance with ISO Quality Regulation 17025 and possess the most advanced LIMS system in the area of managing laboratory data.

D9-THC -> CAS Number: 1972-08-3
http://www.sigmaaldrich.com/catalog...=1972-08-3&D7=0&D10=&N25=0&N1=S_ID&ST=RS&F=PR

THCA -> CAS Number: 23978-85-0
http://www.sigmaaldrich.com/catalog...&D7=0&D10=23978-85-0&N1=S_ID&ST=RS&N25=0&F=PR

CBD-> CAS Number: 13956-29-1
http://www.sigmaaldrich.com/catalog...&D7=0&D10=13956-29-1&N1=S_ID&ST=RS&N25=0&F=PR

CBDA-> CAS Number: 1244-58-2
http://www.sigmaaldrich.com/catalog...2&D7=0&D10=1244-58-2&N1=S_ID&ST=RS&N25=0&F=PR

CBN-> CAS Number: 521-35-7
http://www.sigmaaldrich.com/catalog...-7&D7=0&D10=521-35-7&N1=S_ID&ST=RS&N25=0&F=PR

D8-THC-> CAS Number: 5957-75-5
http://www.sigmaaldrich.com/catalog...5&D7=0&D10=5957-75-5&N1=S_ID&ST=RS&N25=0&F=PR

CBG-> CAS Number: 2808-33-5
https://biochem.thc-pharm.de/product_info.php?cPath=5&products_id=40

CBC ->CAS Number: 20675-51-8
http://www.chemindustry.com/chemicals/1044396.html

We’ll post some results.
Peace.

 

[mofeta]

The lab is Milouda & Migal Laboratories (www.migal.org.il) with (HP) Agilent Tech 7890A GC with 5975C VLMSD and TD.
This Lab develops new protocols for analysis. They will bring new cannabinoid GM/MS analysis protocol to Dr.Mechoulam Lab.
Each test is done 3 times to confirm results.
The laboratories operate in accordance with ISO Quality Regulation 17025 and possess the most advanced LIMS system in the area of managing laboratory data.

Excellent! You are sure to get accurate, precise results. Those guys are well-known experts at analysis of biological materials, and are particularly good at devising methods of doing so. I'm not surprised that Mechoulam chose them.

What are your research goals? Are you doing pure research or do you have some practical goal in mind?

Thanks in advance.

mofeta

 

[Macola]

For those of you looking for reference materials, there are plenty of places on the internet that offer them. Here are a couple of examples:

I'm not sure if all of these stock cannabinoids but my chemist friend said this is a good starting list when searching for standards.

Alfa Aesar
Aurora Fine Chemicals
Biosynth
Cayman Chemical
Cerilliant http://www.cerilliant.com/products/catalog.aspx
Grace Davison
Lipomed
PerkinElmer
Sigma Aldrich
Spectrum
Steraloids
THC Pharm
Tocris Bioscience http://www.tocris.com/
Toronto Research Chemicals
U.S. Pharmacopeia

 

[SacredBreh]

Great thread idea!

Great thread idea!

Seems we have some Mental Giants in the boat.

Thanks for sharing your specialized knowledge.

Peace

 

[Gray Wolf]

Does it have an fid[flame inonization] dectector or tcd [thermal condutivity] these two dectors are the most common the fid will work great for cannabinoid analysis.

My package arrived and it appears in good shape, from a university lab.

It came with both a FID and a hot wire detector and looks like first thing I will have to dig up a dot matrix printer that will interface with it, as well as an older computer. I forgot about that aspect of 1988 technology!

I think my 386 in the attic will work and GG has a line on a printer with the correct protocol. Joe is currently accessing the tests that we need to run, so we can put an accessory list together and get it rolling.

Waiting for a return call from my geekmiester ex-bro-law, to see if he can interface a modern printer and computer, so we are heading at it from both ends.

Any of ya'll have any insight on interfacing modern printing and computing equipment to a PE 8500?