开发一种高效液相色谱-电喷雾质谱分析法，用于特异性和灵敏地定量新型免疫抑制大环内酯类药物40-O-(2-羟乙基)雷帕霉素。

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.

作者信息

Segarra I, Brazelton T R, Guterman N, Hausen B, Jacobsen W, Morris R E, Benet L Z, Christians U

机构信息

Department of Biopharmaceutical Sciences, University of California at San Francisco, 94143-0446, USA.

出版信息

J Chromatogr B Biomed Sci Appl. 1998 Dec 11;720(1-2):179-87. doi: 10.1016/s0378-4347(98)00426-5.

DOI:10.1016/s0378-4347(98)00426-5

PMID:9892080

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.

摘要

我们的目标是开发一种快速、灵敏且特异的检测方法，用于定量移植患者血液中免疫抑制性大环内酯类药物40-O-(2-羟乙基)雷帕霉素（SDZ-RAD）。通过固液萃取从血液中提取SDZ-RAD。使用高效液相色谱-电喷雾质谱法对SDZ-RAD及其内标28,40-二乙酰雷帕霉素进行定量。该检测方法在0.1至100微克/升范围内呈线性（r2 = 0.99）。SDZ-RAD的平均回收率为83%，内标的平均回收率为80.5%。平均日间精密度为8.0%。提取的样品在20℃下至少稳定48小时，SDZ-RAD血液样品在-80℃下至少稳定六个月。