High-performance liquid chromatographic separation and ultraviolet detection of prostaglandins, oxidized by pyridinium dichromate
1983; Elsevier BV; Volume: 282; Linguagem: Inglês
10.1016/s0021-9673(00)91620-0
ISSN1873-3778
Autores Tópico(s)Analytical Methods in Pharmaceuticals
ResumoA rapid UV derivatization procedure has been developed which allows complete separation of the prostaglandins E1, E2, A1, A2, B1 and B2 in less than 12 min. on a C18 reversed-phase column with an acetonitrile-10 mM aq. formic acid gradient as the mobile phase. With pyridinium dichromate in acetonitrile, the prostaglandins could be completely and selectively oxidized to their corresponding 15-oxo derivatives in 8 min. The oxidized prostaglandins were found to have UV maxima at 228 nm (PGE1, PGE2, PGA1 and PGA2) and 298 nm (PGB1 and PGB2). This means that prostaglandins which otherwise needs to be chromatographed by isocratic elution at 192 nm, where the detector noise is considerable, now can be analyzed by gradient elution at 228 nm. Prolonged reaction of PGE1 and PGE2 with pyridinium dichromate gave rise to a second product, probably by oxidation of the non-allylic 11-hydroxyl group, but within 8 min peak heights were less than 3% relative to the major product. The smallest detectable amount has been determined to be 30–80 pmol.
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