I am running about 20 samples in an Agilent HPLC system (standards + experimental samples), and I seem to only get peak tailing in 2 samples only in. Analyzing a butyrate and acetate mixtures, using a biorad HPX-87H analytical column that is roughly new. The acetate peak that i am interested in is the only one that has peak tailing. Using 5mM H2SO4 for the mobile phase.
Wash column properly first then slightly change in flow rate. also check the proper wave length of detection.
For proper washing, run the solvent before and after the sample. The wavelength has to be accurate accordingly.
Condition the column before analysis. If problem still persists then column chemistry is responsible as well as method developed for analysis of butyrate and acetate mixture.
Sorry to answer a question with a question, but is the acetate at relatively low concentration in the 2 samples where you see the tailing? If so you probably have a matrix effect occurring since you apparently do not see tailing in the standards and other samples. Depending on the concentration of the acetate you might try spiking those samples with a concentration near the top end of your calibration and see if the tailing is significantly diminished; if so then it almost certainly is your matrix.
It could also be that this one sample consumes the 5 mM sulfuric acid because it is basic. You may increase the concentration of sulfuric acid in the mobile phase to 10 mM or neutralize the sample beforehand.
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