Sensitive and specific quantification of sirolimus (rapamycin) and its metabolites in blood of kidney graft recipients by HPLC/electrospray-mass spectrometry.
Sensitive and specific quantification of sirolimus (rapamycin) and its metabolites in blood of kidney graft recipients by HPLC/electrospray-mass spectrometry.
复制标题
通过 HPLC/电喷雾质谱法对肾移植受者血液中的西罗莫司（雷帕霉素）及其代谢物进行灵敏且特异的定量。
作者：
Frank Streit;Uwe Christians;H. Schiebel;K. Napoli;Annette Linck;Barry D Kahan;Karl
西罗莫司（雷帕霉素）具有大环内酯类结构，正在进行器官移植后免疫抑制剂的临床研究。建立了血液中西罗莫司的高效液相色谱/质谱分析方法。以28- o -乙酰西罗莫司为内标。采用C18柱提取血样。提取液注入高效液相色谱系统，用甲醇/1%甲酸（体积比90/10）从150 X 4 mm C18分析柱中等比洗脱。高效液相色谱系统与电喷雾界面的三级四极质谱联用，检测正离子。在1 mL血液中的定量限为0.25微克/L，在250微克/L以内血液中的校准曲线呈线性。血中回收率为88 +/- 26%，在1微克/L和15微克/L时的测定间变异率分别为19%和9.3%。肾移植患者血液中检测到羟基、二羟基、去甲基、二甲基西罗莫司及西罗莫司。
Sirolimus (rapamycin) has a macrolide structure and is under clinical investigation as an immunosuppressant after organ transplantation. An HPLC/mass spectrometry assay to quantify sirolimus in blood was developed. 28-O-Acetyl sirolimus was used as internal standard. Blood samples were extracted with C18 columns. The extracts were injected into an HPLC system and isocratically eluted with methanol/1% formic acid (90/10 by vol) from a 150 X 4 mm C18 analytical column. The HPLC system was connected to a triple-stage quadrupole mass spectrometer with an electrospray interface and positive ions were detected. The limit of quantification in 1 mL of blood was 0.25 microgram/L and the calibration curve in blood was linear up to 250 microgram/L. The recovery from blood was 88 +/- 26% and interassay variation at 1 microgram/L was 19% and at 15 microgram/L 9.3%. Hydroxy, dihydroxy, demethyl, and didemethyl sirolimus as well as sirolimus were detected in blood of kidney graft patients.
新型强效免疫抑制剂雷帕霉素的临床前评估。
影响因子：
6.2
作者：
Kahan,BD;Chang,JY;Sehgal,SN
通讯作者：
Sehgal,SN
环孢素：免疫抑制治疗的基础——现在和未来。
影响因子：
0.9
作者：
Kahan,BD
通讯作者：
Kahan,BD
影响因子：
56.9
作者：
SCHREIBER, SL
通讯作者：
SCHREIBER, SL