Determination of immunosuppressive drugs in human urine and serum by surface-assisted laser desorption/ionization mass spectrometry with dispersive liquid-liquid microextraction

被引:14
作者
Chen, Pin-Shiuan [1 ]
Cheng, Yu-Han [1 ]
Lin, Sheng-Yu [1 ]
Chang, Sarah Y. [1 ]
机构
[1] Natl Kaohsiung Normal Univ, Dept Chem, Kaohsiung 824, Taiwan
关键词
Surface-assisted laser desorption/ionization mass spectrometry; Dispersive liquid-liquid microextraction; Immunosuppressive drugs; Urine sample; Serum sample; SOLID-PHASE EXTRACTION; MICELLAR ELECTROKINETIC CHROMATOGRAPHY; HUMAN WHOLE-BLOOD; CYCLOSPORINE-A; LC-MS/MS; SIMULTANEOUS QUANTIFICATION; TRACE ANALYSIS; LC/ESI-MS/MS; HUMAN PLASMA; PERFORMANCE;
D O I
10.1007/s00216-015-9145-9
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A rapid and sensitive method for the determination of immunosuppressive drugs through surface-assisted laser desorption/ionization mass spectrometric detection (SALDI/MS) was developed. Colloidal Pd and alpha-cyano-4-hydroxycinnamic acid (CHCA) were used as the SALDI co-matrix. To eliminate interference and enhance the sensitivity, dispersive liquid-liquid microextraction (DLLME) was employed to extract the immunosuppressive drugs from the aqueous solutions. Under optimal extraction and detection conditions, calibration curves for cyclosporine and everolimus in aqueous solutions were linear over a concentration range from 0.01 to 1.20 mu M. For sirolimus, the linear concentration range of the calibration curve was from 0.05 to 2.00 mu M. The limits of detection (LODs) were calculated to be 3, 3, and 14 nM for cyclosporine, everolimus, and sirolimus, respectively. The enrichment factors of DLLME were calculated to be 108, 122, and 101 for cyclosporine, everolimus, and sirolimus, respectively. This novel method was successfully applied for the determination of immunosuppressive drugs in human urine and serum samples.
引用
收藏
页码:629 / 637
页数:9
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