Sioufi A, Leroux F, Sandrenan N
J Chromatogr. 1983 Jan 14;272(1):103-10. doi: 10.1016/s0378-4347(00)86107-1.
A method for the determination of metoprolol at concentrations down to 10 ng/ml in human plasma is described. After addition of oxprenolol as internal standard, both compounds are extracted into diethyl ether--dichloromethane (4:1, v/v) at basic pH, transferred into an acidic aqueous solution and back-extracted at basic pH into diethyl ether--dichloromethane. They are then derivatized with heptafluorobutyric anhydride. The derivatives are quantitatively determined by gas chromatography using a 63Ni electron-capture detector. The linearity was demonstrated, and the technique was formally validated in the concentration range 10-500 ng/ml. The technique was applied in a study of the bioavailability of metoprolol after oral administration to man; mean plasma concentrations are reported.
本文描述了一种测定人血浆中低至10 ng/ml美托洛尔浓度的方法。加入氧烯洛尔作为内标后，在碱性pH条件下将两种化合物萃取到乙醚-二氯甲烷（4:1，v/v）中，转移至酸性水溶液中，再在碱性pH条件下回萃取到乙醚-二氯甲烷中。然后用七氟丁酸酐进行衍生化。使用63Ni电子捕获检测器通过气相色谱法定量测定衍生物。证明了该方法的线性，并在10-500 ng/ml浓度范围内对该技术进行了正式验证。该技术应用于一项关于美托洛尔口服给药后人的生物利用度的研究；报告了平均血浆浓度。
