Rouan M C, Campestrini J, Lecaillon J B, Dubois J P, Lamontagne M, Pichon B
Laboratoires Ciba-Geigy, Biopharmaceutical Research Centre, Rueil-Malmaison, France.
J Chromatogr. 1988 Dec 2;456(1):45-51. doi: 10.1016/0021-9673(86)80005-x.
Liquid-solid extraction on disposable extraction columns (DECs) and liquid chromatography can be combined in a completely automated analyser. The Gilson ASPEC system was used to develop a procedure for the determination of CGP 6140 in plasma. Both sample preparation via C8 Bond-Elut DECs and injection were fully automatic. The fully automated system prepared the samples by performing the same operations as for a manual procedure. The DEC was first wetted with methanol, then with water. A 400-microliters volume of plasma and 40 microliters of the internal standard solution, diluted with 1 ml of water, were applied to the DEC, rinsed with 10(-2) mol/l dipotassium hydrogenphosphate and eluted from the DEC with 300 microliters of acetonitrile-methanol (50:50, v/v). The eluting strength of the eluate was reduced by dispensing 1 ml of water into each vial prior to direct injection into a Spherisorb ODS column via a 1-ml loop. This allowed the reconcentration of the extracted compounds on the top of the column, as they were injected in a large volume of solvent of lower eluting strength than the mobile phase [acetonitrile-methanol-4 x 10(-3) mol/l ammonia solution (54.5:5:40.5, v/v/v)]. Reproducibility results are presented.
一次性萃取柱（DEC）上的液固萃取与液相色谱可结合在一个全自动分析仪中。使用吉尔森ASPEC系统开发了一种测定血浆中CGP 6140的方法。通过C8 Bond-Elut DEC进行的样品前处理和进样均为全自动。该全自动系统通过执行与手动操作相同的步骤来制备样品。首先用甲醇润湿DEC，然后用水润湿。将400微升血浆和40微升用1毫升水稀释的内标溶液加到DEC上，用10⁻²摩尔/升磷酸氢二钾冲洗，并用300微升乙腈 - 甲醇（50:50，v/v）从DEC上洗脱。在通过1毫升定量环直接进样到Spherisorb ODS柱之前，向每个样品瓶中加入1毫升水，以此降低洗脱液的洗脱强度。这样可以使萃取的化合物在柱顶重新富集，因为它们是用比流动相[乙腈 - 甲醇 - 4×10⁻³摩尔/升氨溶液（54.5:5:40.5，v/v/v）]洗脱强度低的大量溶剂进样的。文中给出了重现性结果。
