Cuisinaud G, Terrier M, Ferry N, Proust S, Sassard J
J Chromatogr. 1985 May 31;341(1):97-104. doi: 10.1016/s0378-4347(00)84013-x.
A sensitive, selective and easy to use high-performance liquid chromatographic method for the determination of cicletanide, a new diuretic, in plasma, red blood cells, urine and saliva is described. After extraction of cicletanide together with an internal standard with diethyl ether, or diethyl ether-n-hexane (20:80) for urine, the sample extracts are chromatographed with water-methanol-acetic acid (50:50:0.3) as eluent on to a Nucleosil C18 column. Both compounds are detected by their ultraviolet absorption at 280 nm. The calibration graph was linear between 0.2 and 20 micrograms/ml for plasma and between 0.2 and 5 micrograms/ml for the other biological fluids. The sensitivity limit was 20 ng/ml for plasma, red blood cells and saliva and 30 ng/ml for urine. The coefficients of variation of the between-day assays did not exceed 4.6% in plasma, 8.3% in red blood cells, 7.8% in urine and 4.2% in saliva for the lowest concentrations studied. The application of the method to a pharmacokinetic study of cicletanide after a single oral therapeutic dose in humans is reported.
本文描述了一种灵敏、选择性好且易于使用的高效液相色谱法,用于测定血浆、红细胞、尿液和唾液中的新型利尿剂西氯他宁。用乙醚或尿液用乙醚 - 正己烷(20:80)将西氯他宁与内标一起萃取后,样品萃取液以水 - 甲醇 - 乙酸(50:50:0.3)作为洗脱剂在Nucleosil C18柱上进行色谱分析。两种化合物均通过其在280 nm处的紫外吸收进行检测。血浆的校准曲线在0.2至20微克/毫升之间呈线性,其他生物流体的校准曲线在0.2至5微克/毫升之间呈线性。血浆、红细胞和唾液的检测限为20纳克/毫升,尿液的检测限为30纳克/毫升。在所研究的最低浓度下,日间测定的变异系数在血浆中不超过4.6%,在红细胞中不超过8.3%,在尿液中不超过7.8%,在唾液中不超过4.2%。报道了该方法在人体单次口服治疗剂量后西氯他宁药代动力学研究中的应用。