Joseph Jack Kirkland answered questions from Gert Desmet on his pioneering career in high performance liquid chromatography
Gert Desmet: How did you enter the field of chromatography?
Joseph Jack Kirkland: In the late 1950s I began to use gas chromatography (GC) to solve problems relating to agricultural products that were being
developed at DuPont. This effort was triggered by interactions with DuPont's Dr. Steve Dal Nogare, who started the early studies
in GC, especially in programmed temperature operation. GC analyses proved to be quite useful, but there were many compounds
of interest to DuPont that were not volatile and could not be separated by this technique.
In some cases, I was able to derivatize these materials to produce structures that were sufficiently volatile for GC analysis,
but many problems still remained that needed a solution. Around 1960, I attempted liquid chromatography (LC) separations of
some nonvolatile compounds using large-particle silica gel columns as the separating medium, a low pressure pump, and a refractometer
as a detector. Crude separations resulted, but it was too slow, poorly reproducible, and very frustrating. I really did not
know enough to create the desired result. Therefore, this project was not pursued further. However, in 1964, when I was visiting
Europe, during a trip to Eindhoven, The Netherlands, I came across Dr. Joseph (J.F.K.) Huber in a laboratory performing what
we now call high performance liquid chromatography (HPLC).
Figure 1: Jack Kirkland in his laboratory in 1960.
Huber was using a constant-pressure pump (1000 psi), a small diameter column with ~50 Ám diatomaceous earth particles, and
an ultraviolet (UV) spectrometer that had been converted into a crude detector. With this arrangement, Huber was demonstrating
remarkable (for that time) separations of nonvolatile compounds using a liquid–liquid chromatographic technique. This visit
was so interesting that on my return to DuPont, I approached my supervisor and pleaded for the time and resources to begin
a program into researching HPLC technology. This request was approved and I then started to develop the materials that were
needed to make the technique routine. To improve the technology, I believed that a better column packing was required, together
with a reliable and highly sensitive UV detector. Both of these items were subsequently developed, put into use, and a patent
and papers on them published.
Perspectives in Modern HPLC: Michael W. Dong is a senior scientist in Small Molecule Drug Discovery at Genentech in South San Francisco, California. He is responsible for new technologies, automation, and supporting late-stage research projects in small molecule analytical chemistry and QC of small molecule pharmaceutical sciences. LATEST: Seven Common Faux Pas in Modern HPLC