Sioufi A, Pommier F, Mangoni P, Gauron S, Metayer J P
J Chromatogr. 1981 Mar 13;222(3):429-35. doi: 10.1016/s0378-4347(00)84143-2.
A method for the determination of unconjugated phentolamine at concentrations down to 5 ng/ml in human plasma, and of free and total (free plus conjugated) phentolamine down to 25 ng/ml in urine is described. After addition of 2-[N-(p-chlorophenyl)-N-(m-hydroxyphenyl)-aminomethyl]-2-imidazoline as internal standard, both compounds are extracted into benzene-ethyl acetate (1:1, v/v) at pH 10, transferred into an acidic aqueous solution and back-extracted at pH 10 into benzene-ethyl acetate. They are then derivatized with N-heptafluorobutyrylimidazole. The derivatives are determined by gas chromatography using a 63Ni electron-capture detector. In urine, total (free plus conjugated) phentolamine is determined after enzymatic hydrolysis. The technique was applied for the study of the plasma concentrations and urinary elimination after oral administration to man.
本文描述了一种测定人血浆中低至5 ng/ml的非结合酚妥拉明以及尿液中低至25 ng/ml的游离和总（游离加结合）酚妥拉明的方法。加入2-[N-(对氯苯基)-N-(间羟基苯基)-氨基甲基]-2-咪唑啉作为内标后，两种化合物在pH 10条件下被萃取到苯 - 乙酸乙酯（1:1，v/v）中，转移至酸性水溶液中，然后在pH 10条件下再萃取回苯 - 乙酸乙酯中。接着它们用N - 七氟丁酰咪唑进行衍生化。衍生物通过使用63Ni电子捕获检测器的气相色谱法进行测定。在尿液中，总（游离加结合）酚妥拉明在酶促水解后进行测定。该技术应用于人体口服给药后的血浆浓度和尿排泄研究。
