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Development of a high-performance liquid chromatographic–electrospray mass spectrometric assay for the specific and sensitive quantification of the novel immunosuppressive macrolide 40-O-(2-hydroxyethyl)rapamycin |
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| Authors: | Ignacio Segarra Timothy R Brazelton Natalya Guterman Bernard Hausen Wolfgang Jacobsen Randall E Morris Leslie Z Benet and Uwe Christians |
| Institution: | a Department of Biopharmaceutical Sciences, University of California at San Francisco, San Francisco, CA 94143-0446, USA b Laboratory of Transplantation Immunology, Department of Cardiothoracic Surgery, Stanford University Medical School, Stanford, CA 94305-5247, USA |
| Abstract: | It was our objective to develop a rapid, sensitive and specific assay to quantify the immunosuppressive macrolide 40-O-(2-hydroxyethyl)rapamycin (SDZ-RAD) in blood of transplant patients. SDZ-RAD was extracted from blood by solid–liquid extraction. SDZ-RAD and its internal standard 28,40-diacetyl rapamycin were quantified using HPLC–electrospray MS. The assay was linear from 0.1 to 100 μg/l (r2=0.99). The mean recovery was 83% for SDZ-RAD and 80.5% for the internal standard. The mean day-to-day precision was 8.0%. Extracted samples were stable at 20°C for at least 48 h and SDZ-RAD blood samples at −80°C for at least six months. |
| Keywords: | 40-O-(2-Hydroxyethyl)rapamycin |
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