Establishment of a candidate reference measurement procedure for the quantification of cyclosporine A,tacrolimus,sirolimus and everolimus in whole blood by ID-LC-MS/MS
10.3760/cma.j.cn114452-20220118-00026
- VernacularTitle:ID-LC-MS/MS法同时测定全血中环孢素A、他克莫司、西罗莫司和依维莫司候选参考方法的建立
- Author:
Qingzhang ZENG
1
;
Tianjiao ZHANG
;
Qichen LONG
;
Lizi JIN
;
Li ZHANG
;
Chuanbao ZHANG
Author Information
1. 北京医院 国家老年医学中心 国家卫生健康委临床检验中心 中国医学科学院老年医学研究院 中国医学科学院北京协和医学院，北京100730
- Keywords:
Tandem mass spectrometry;
Cyclosporine A;
Tacrolimus;
Sirolimus;
Everolimus
- From:
Chinese Journal of Laboratory Medicine
2022;45(5):472-477
- CountryChina
- Language:Chinese
-
Abstract:
Objectives:To establish a candidate reference measurement procedure based on isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) for cyclosporin A, tacrolimus, sirolimus, and everolimus measurements in human whole blood.Methods:The isotope labeled cyclosporine A, tacrolimus, sirolimus, and everolimus were selected as the internal standards. Samples were accurately weighed while protein precipitation and solid phase extraction were selected for the sample preparation. The standard curve method was applied for quantification. The ultra-high liquid chromatography coupled with triple quadrupole mass spectrometer was used for analysis. The specificity, matrix effect, detection limit, quantification limit, precision, accuracy, and uncertainty of the method were evaluated.Results:The method showed good selectivity and specificity. No apparent interferences or matrix effects were found in the target analyte measurements. The detection limits and quantification limits of cyclosporin A, tacrolimus, sirolimus and everolimus met clinical requirements. Intra-batch coefficients of variation ( CV) were from 1.4% to 1.8% for CSA, from 1.7% to 2.8% for TAC, from 1.3% to 3.7% for SRL and from 2.3% to 3.2% for EVR, and total CVs were from 1.8% to 2.9% for CSA, from 1.7% to 3.8% for TAC, from 2.6% to 4.7% for SRL and from 3.5% to 4.6% for EVR. The relative recoveries were from 97.9% to 100.3% for CSA, from 98.4% to 103.1% for TAC, from 99.4% to 102.0% for SRL and from 98.3% to 99.4% for EVR, and the relative expanded uncertainties at four concentrations were from 4.2% to 4.4% for CSA, from 1.5% to 2.4% for TAC, from 4.4% to 4.9% for SRL and from 2.2% to 2.7% for EVR. Conclusion:A candidate reference measurement procedure for the cyclosporine A, tacrolimus, sirolimus, and everolimus in human whole blood was established by ID-LC-MS/MS.
