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Simultaneous on-line extraction and analysis of sirolimus (rapamycin) and ciclosporin in blood by liquid chromatography–electrospray mass spectrometry

1999; Elsevier BV; Volume: 721; Issue: 2 Linguagem: Inglês

10.1016/s0378-4347(98)00463-0

1872-812X

Gabriele Kirchner, C Vidal, Wolfgang Jacobsen, Anke Franzke, Katrin Hallensleben, Uwe Christians, Karl‐Friedrich Sewing,

Signaling Pathways in Disease

We developed a sensitive and specific semi-automated liquid chromatography–electrospray mass spectrometric (HPLC–ESI-MS) assay for the simultaneous quantification of sirolimus and ciclosporin in blood. Following a simple protein precipitation step, the supernatants were injected into the HPLC system and extracted on-line. After column switching, the analytes were backflushed from the extraction column onto the analytical narrow-bore column and eluted into the ESI-MS system. The assay was linear from 0.4 to 100 μg/l sirolimus and from 2 to 1500 μg/l ciclosporin. The mean recoveries of sirolimus and ciclosporin were 98 and 96%, respectively. The mean interday precision/accuracy was 8.6%/−4.8% for sirolimus and 9.3%/−2.9% for ciclosporin.