In-situ derivatization of ibuprofen in equine urine using the apex prosep precolumn separation inlet (psi) and the hp 5973 msd system

In-situ Derivatization of Ibuprofen in Equine Urine Using the APEX ProSep 800 XT Precolumn Separation Solution
The analysis of drugs and drug metabolites is often a challenge for the chemist. This is due to the Inlet (PSI) provides the correct reaction physical and chemical properties of many drugs, but environment to perform this derivatization can also be attributed to the matrix of the sample, e.g. procedure. The sample and derivatizing agent are f blood, urine or other biological fluid. Both added to an autosampler vial and then placed in characteristics make this type of analysis very time the autosampler tray. The HP 7683 ALS then consuming and in many cases levels of detection are mixes the sample and derivatizing agent with a 6 compromised due to matrix related issues. Derivatization in the form of methylation is often a necessary sample preparation step to physically injected into the PSI-GC/MSD System. The alter the compounds of interest. This process is performed in order to change specific compounds of temperature program providing both the proper interest so they will be amenable to gas reaction temperature and long thermal residence time required carrying out the methylation reaction; an environment a standard split/splitless In this example, derivatization of Ibuprofen inlet cannot provide. The PSI technique provides (Figure 1.) found in equine urine samples is typically significant time and cost savings when compared prepared on the bench prior to placing the sample with traditional bench sample preparation and into the autosampler vial. This step, although derivatization methods. The 50µL injection size necessary for gas chromatographic analysis, is very also increases the sensitivity by more than an time intensive. In addition, the sample matrix can order of magnitude when compared with 1µL injection methodologies. The data presented here shows a comparison of a bench-derivatized standard containing Ibuprofen to a ProSep 50µL Derivatizing Agent
Figure 1. Methylation reaction of
In-situ Derivatization of Ibuprofen in Equine Urine Using The APEX ProSep™ Precolumn Separation Inlet (PSI) and the HP 5973 MSD System INNOVATIONS IN GAS CHROMATOGRAPHY …
Figure 3. Bench derivatized Ibuprofen.
Figure 4. ProSep 50µL injection of Ibuprofen and
derivatization agent.
APEX Technologies, Inc. would like to recognize Dr. Wayne Skinner, University of California - Davis for his continued work in the area of in-situ derivatization and low-level detection of drugs in biological matrices APEX Technologies shall not be liable for errors contained
herein or for incidental or consequential damages in
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connection with the furnishing, performance or use of this


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are subject to change without notice.

Copyright 1999
APEX Technologies, Inc.

All rights reserved. Reproduction and adaptation is prohibited.
Printed in the U.S.A. October-1999


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