使用先进的自动样品处理单元通过液相色谱法测定全血中的环孢素。

Liquid chromatographic determination of cyclosporine in whole blood with the advanced automated sample processing unit.

作者信息

Kabra P M, Wall J H

出版信息

J Chromatogr. 1987 Jan 9;385:305-10. doi: 10.1016/s0021-9673(01)94645-x.

Abstract

We describe a rapid, precise, cost-effective, and accurate isocratic liquid chromatographic (LC) procedure for determining cyclosporine in whole blood. The cyclosporine is extracted from 0.5 ml of whole blood together with 200 micrograms of cyclosporin D, added per liter as internal standard, by using an Advanced Automated Sample Processing (AASP) unit. The on-line solid-phase extraction is performed on an octasilane sorbent cartridge which is interfaced with a Perkin-Elmer 83 X 4.6 mm I.D. cartridge column, packed with 3-micron octadecyl packing. The column is eluted with a mobile phase containing acetonitrile-water (13:7) at a flow-rate of 1.0 ml/min at a column temperature of 70 degrees C. The column effluent is monitored at 210 nm. The absolute recovery of cyclosporine exceeded 87% and the linearity extended up to 2000 micrograms/l. Within-run and day-to-day coefficients of variation were less than 8%. The correlation between AASP-LC and manual Bond-Elut extraction-LC method was excellent (r = 0.97).

摘要

我们描述了一种快速、精确、经济高效且准确的等度液相色谱（LC）方法，用于测定全血中的环孢素。通过使用高级自动样品处理（AASP）装置，从0.5 ml全血中提取环孢素，同时加入每升200微克的环孢素D作为内标。在线固相萃取在一个八硅烷吸附剂柱上进行，该柱与内径为4.6 mm的Perkin-Elmer 83柱相连，填充3微米的十八烷基填料。在柱温70℃下，以1.0 ml/min的流速用含有乙腈-水（13:7）的流动相洗脱该柱。在210 nm处监测柱流出物。环孢素的绝对回收率超过87%，线性范围扩展至2000微克/升。批内和日间变异系数均小于8%。AASP-LC法与手动Bond-Elut萃取-LC法之间的相关性极佳（r = 0.97）。