title: 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.
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 microg/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 degrees C for at least 48 h and SDZ-RAD blood samples at -80 degrees C for at least six months.
authors.affiliation: Department of Biopharmaceutical Sciences, University of California at San Francisco, 94143-0446, USA.
authors.forename: I
authors.initials: I
authors.lastname: Segarra
authors.forename: T R
authors.initials: TR
authors.lastname: Brazelton
authors.forename: N
authors.initials: N
authors.lastname: Guterman
authors.forename: B
authors.initials: B
authors.lastname: Hausen
authors.forename: W
authors.initials: W
authors.lastname: Jacobsen
authors.forename: R E
authors.initials: RE
authors.lastname: Morris
authors.forename: L Z
authors.initials: LZ
authors.lastname: Benet
authors.forename: U
authors.initials: U
authors.lastname: Christians
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D000068338:Everolimus; D006801:Humans; D007166:Immunosuppressive Agents / Q000097:blood*; D013058:Mass Spectrometry / Q000379:methods*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D020123:Sirolimus / Q000031:analogs & derivatives* / Q000097:blood
chemical_list: D007166:Immunosuppressive Agents; D000068338:Everolimus; D020123:Sirolimus