HPLC Sample Derivatization - 2butoxyethanol

[hello345]

Hi All

I am currently trying to develop a method for the analysis of 2-butoxyethanol (EGMBE). There are a limited number of methods within the literature for this and the ones which are available involve the use of GC-MS or HPLC with UV detection following sample derivatization. Unfortunately we don't have a GC-MS system in our laboratory and we were hoping to avoid a derivatization step.

We recently purchased a charged aerosol detector in our laboratory and I was hoping this may be a viable option for analysis when combined with our HPLC Dionex system. However, it seems 2-butoxyethanol may be a little too volatile to be analysed using this detector.

I don't have very much experience with sample preparation techniques, however I was wondering if anyone would know if it is possible to derivatize a sample to make it less volatile, more specifically 2-butoxyethanol?

Any other comments or advice would also be greatly appreciated

Many Thanks

[X]

Please see the paper below using pre-column derivatization with 1-anthroylnitrile:

Sensitive determination of alkoxyethanols by pre-column derivatization with 1-anthroylnitrile and reversed-phase high-performance liquid chromatography.
Yoshikawa M, Tani C.
J Chromatogr A. 2003 Jul 11;1005(1-2):215-21.

Abstract
A new method for simultaneous determination of alkoxyethanols (2-methoxyethanol, 2-ethoxyethanol, 2-isopropoxyethanol, and 2-butoxyethanol) by high-performance liquid chromatography (HPLC) with fluorescence detection has been developed. The alkoxyethanols and an internal standard (2-phenoxyethanol) were derivatized by treatment with 1-anthroylnitrile to give the anthroyl esters. The esterification was completed in 30 min in the presence of quinuclidine as base catalyst at room temperature. After stopping the reaction, an aliquot of the final solution was injected into the HPLC. The resulting anthroyl esters of the alkoxyethanols and the internal standard were separated on a C18 reversed-phase column with acetonitrile-water-acetic acid (65:35:0.1, v/v) as the mobile phase and detected fluorimetrically at excitation and emission wavelengths of 360 nm and 460 nm, respectively. The detection limits of the derivatives as alkoxyethanols at a signal-to-noise ratio of 3 were in the range of 1-3 pg per injection. The minimal amounts of alkoxyethanols derivatized in the reaction mixture for derivatization to determine the limits of detection were approximately 0.5 ng. This HPLC method was applied to the determination of some of alkoxyethanols in the air of the workplace where the thinner containing alkoxyethanols was used for painting.

[hello345]

Thank you very much for the reply.

I have a copy of this paper and the derivatization process detailed within it is something I have considered using. We don't have a fluorescence detector and therefore would still be using the charged aerosol detector after derivatization. My hope would be that the derivatization process and ultimately the final product (1-butoxyethanol anthroyl ester) would be less volatile and therefore enable detection using the CAD.

Many Thanks

[Consumer Products Guy]

You're making this WAY too tough.

2-butoxyethanol has been a common solvent in window cleaners and such. We've assayed 2-butoxyethanol for decades.

Use GC with FID, and we typically dissolve in dimethylformamide and make trimethylsilyl derivative using BSTFA or similar, and use a nonpolar capillary such as DB-1 or DB-5.

We've also run without derivatization on a PEG capillary, but haven't tried on a different polar capillary such as DB-624.

[hello345]

Thanks for the reply

As mentioned in my original post we don't have any GC-MS capabilities in our laboratory and therefore this isn't an option at this moment in time (I should really have stated we have no GC capabilities at all). As we recently acquired the new charged aerosol detector we were wanting to determine if we could use HPLC for analysis - although it isn't looking likely.

Maybe we will just have to invest in a new piece of equipment.

Thanks Again

[Consumer Products Guy]

I should really have stated we have no GC capabilities at all.
Maybe we will just have to invest in a new piece of equipment.

There's an old saying that I just made up: "it's tough to cook an egg with a water faucet". In this case you're trying to fit a GC assay onto an HPLC. Tell your boss that your lab is half a lab (at best) without some GC.

Are you perhaps in a pharmaceutical lab where people and regulatory agencies think HPLC is for everything?

[hello345]

Yes having no GC does make research somewhat troublesome at times.

No I am carrying out research for a university. The department I am in specialises in scale control for the petroleum industry.

The department wants to focus on the development of analytical methods for the analysis of chemicals commonly used to control the formation of scale offshore, primarily scale inhibitors and 2-butoxyethanol. However the only instruments available for use are an HPLC with UV/CAD/Conductivity detection capabilities and an ICP.

Does anyone know roughly how much a new GC system would cost?

Many thanks

[rb6banjo]

I agree with the others. This is a GC analysis and would be kindergarten for you if you had the right instrumentation.

New, GC's are pretty pricey for an academic lab - even without a mass spectrometer.

If I were you, I would check with some of the second-hand instrument dealers like labx.com or even ebay! There are a couple of Hewlett-Packard (now Agilent Technologies) 5890A's up for bid and the current price is only $500. I have a 5890A in my lab that is 25 years old and still works very well.

[mrussell]

Hi All

I am currently trying to develop a method for the analysis of 2-butoxyethanol (EGMBE). There are a limited number of methods within the literature for this and the ones which are available involve the use of GC-MS or HPLC with UV detection following sample derivatization. Unfortunately we don't have a GC-MS system in our laboratory and we were hoping to avoid a derivatization step.

We recently purchased a charged aerosol detector in our laboratory and I was hoping this may be a viable option for analysis when combined with our HPLC Dionex system. However, it seems 2-butoxyethanol may be a little too volatile to be analysed using this detector.

I don't have very much experience with sample preparation techniques, however I was wondering if anyone would know if it is possible to derivatize a sample to make it less volatile, more specifically 2-butoxyethanol?

Any other comments or advice would also be greatly appreciated

Many Thanks

I just run it by GC-FID. What detections limits are you trying for.