Determination of sirolimus in human whole blood by LC-MS/MS
10.13699/j.cnki.1001-6821.2016.03.019
- VernacularTitle:LC－MS／MS法测定人全血中西罗莫司的浓度研究
- Author:
Qing DING
1
;
Duan-Hao FENG
Author Information
1. 河北北方学院 研究生部
- Keywords:
sirolimus;
HPLC-MS/MS;
pharmacokinetic
- From:
The Chinese Journal of Clinical Pharmacology
2016;(3):254-256
- CountryChina
- Language:Chinese
-
Abstract:
Objective To develop a method for determination of sirolimus in human whole blood by HPLC -MS/MS.Methods The whole blood samples using ascomycins as internal standard were treated with zinc sul-fate and acetonitrile.After precipitation, the supernatant 5μL was injec-ted for analysis.The used column was Extend -C18 column (2.1 mm × 50 mm, 3.5 μm), mobile phase consisted of 10 mmol· L-1 ammonium acetate solution ( A) and methanol ( B) with a gradient elution.The flow rate was 0.4 mL· min -1 , the analyte and internal standard were detec-ted by multiple reaction monitoring scanning in positive ion mode using triple quadrupole mass spectrometer.The specificity , standard curve and lower limitation of quantitation , precision and recovery rate and stability as well as the matrix effect were investigated.Results The linear range of sirolimus was 0.5-100.0 ng · mL-1 ( r=0.998 3 ).The intra-day and inter-day RSD were both less than 10%.The extraction recoveries were 89.7%-91.6%.Conclusion The method is simple, rapid, sen-sitive and accurate for monitoring of whole blood concentration of siroli-mus and the pharmacokinetic study in human body.
