Preparation of urine samples for liquid-chromatographic determination of catecholamines: bonded-phase phenylboronic acid, cation-exchange resin, and alumina adsorbents compared.

We compared results for the liquid-chromatographic determination of free norepinephrine and epinephrine in urine after purifying the catechols by the following methods: (a) acid-washed alumina, (b) weak cation-exchange resin (WCX), (c) a combination of weak cation-exchange resin followed by alumina (WCX-alumina), and (d) commercially available phenylboronic acid adsorbent. We evaluated analytical specificity, sensitivity, recovery, and turnaround time. The WCX-alumina combination produced the most sensitive and specific chromatograms for urinary catecholamines; the other methods took less processing time. Neither WCX nor alumina alone was suitable for routine work because of chromatographic interferences in a significant proportion of urines. The phenylboronic acid method is adequately sensitive and specific for norepinephrine and epinephrine, and samples can be assayed faster. Thus it provides a compromise between the high analytical performance of the WCX-alumina method and the speed of the WCX and alumina methods.