Krogh M, Johansen K, Tønnesen F, Rasmussen K E
Institute of Pharmacy, University of Oslo, Norway.
J Chromatogr B Biomed Appl. 1995 Nov 17;673(2):299-305. doi: 10.1016/0378-4347(95)00273-8.
The potential of solid-phase microextraction in the bioanalysis of drugs is demonstrated. The free concentration of valproic acid in human plasma was determined by equilibrium dialysis at room temperature. To the dialysate was added an internal standard and the pH was adjusted to 2.5. The polymethylsiloxane-coated fused-silica fibre of the solid-phase microextraction device was inserted into the dialysate for 3 min. The sorbed analytes were then thermally desorbed at 210 degrees C in the split-splitless injection port of the gas chromatograph, separated on a Nukol capillary column and detected with a flame ionization detector. The method was shown to be highly reproducible with a detection limit of 1 microgram/ml of free valproic acid in human plasma.
展示了固相微萃取在药物生物分析中的潜力。通过在室温下进行平衡透析来测定人血浆中丙戊酸的游离浓度。向透析液中加入内标并将pH值调至2.5。将固相微萃取装置的聚甲基硅氧烷涂层熔融石英纤维插入透析液中3分钟。然后将吸附的分析物在气相色谱仪的分流/不分流进样口中于210℃进行热解吸，在Nukol毛细管柱上分离并用火焰离子化检测器进行检测。该方法具有高度重现性，人血浆中游离丙戊酸的检测限为1微克/毫升。
