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  • Title: Profiles of prostaglandins A, B, E and F (series I and II) obtained by gas chromatography with multiple-ion detection.
    Author: Rosello J, Tusell J, Gelpi E.
    Journal: J Chromatogr; 1977 Jan 11; 130():65-76. PubMed ID: 856850.
    Abstract:
    A new method is presented for the simultaneous one-step derivatization of prostaglandins A1, A2, B1, B2, E1, E2, F1alpha and F2alpha with N,O-bis(trimethylsilyl)trifluoroacetamide-piperidine. The procedure provides stable and reproducible trimethylsilyl derivatives that show good chromatographic properties on OV-17 and OV-225 columns, and precludes any significant degree of interconversion of the prostaglandins. The prostaglandins F, B and E are determined as the corresponding tetrakis(trimethylsilyl), bis(trimethylsilyl) and 9-enol-tetrakis(trimethylsilyl) derivatives, respectively. The enolization of prostaglandins E proceeds quantitatively only if piperidine is added to the acetamide. This mixture also produces the novel derivative 9-piperidyl-tris(trimethylsilyl)prostaglandin A. Evidence is also presented on the quantitative injection losses due to the type of syringe used (1micronl or 10 micronl). A modified extraction procedure has been applied to samples of human seminal fluid. The procedure, which involves the centrifugation of the samples, allows the recovery of all of the prostaglandins in one fraction, which is then derivatized and screened by combined gas-liquid chromatography-multiple-ion detection techniques in order to identify the individual compounds.
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