Corta E, Bakkali A, Berrueta L A, Gallo B, Vicente F, Gonzalo A, Lucero M L, Orjales A
Department of Analytical Chemistry, Faculty of Sciences, University of the Basque Country, Bilbao, Spain.
J Chromatogr B Biomed Sci Appl. 1999 Apr 30;727(1-2):131-8. doi: 10.1016/s0378-4347(99)00061-4.
A solid-phase extraction (SPE) method for sample clean-up followed by a reversed-phase HPLC procedure for the assay of alinastina (pINN) in biological fluids is reported. The effects of the sample pH, composition of the washing and elution solvents and the nature of the SPE cartridge on recovery were evaluated. The selectivity of SPE was examined using spiked rat urine and plasma samples and the CH and PH cartridges gave rise to the cleanest extracts. The recoveries obtained in spiked rat urine and plasma samples were 91.2+/-2.7 and 99.9+/-2.8%, respectively. The proposed SPE method coupled off-line with a reserved-phase HPLC system with fluorimetric detection was applied to the quantitation of alinastine in real rat urine samples. The analytical method was also applied and validated for the determination of alinastine in dog plasma. The recovery from spiked dog plasma samples using the PH cartridge was around 65%. The within-day and between-day precisions were 7 and 12%, respectively. The detection and quantitation limits in dog plasma were 0.024 and 0.078 microg/ml, respectively.
本文报道了一种用于生物样品净化的固相萃取（SPE）方法，随后采用反相高效液相色谱法测定生物流体中的阿利纳斯汀（国际非专利药品名称）。评估了样品pH值、洗涤和洗脱溶剂组成以及SPE柱性质对回收率的影响。使用加标大鼠尿液和血浆样品检测了SPE的选择性，CH柱和PH柱得到的提取物最纯净。加标大鼠尿液和血浆样品中的回收率分别为91.2±2.7%和99.9±2.8%。所提出的SPE方法与配备荧光检测的反相高效液相色谱系统离线联用，用于实际大鼠尿液样品中阿利纳斯汀的定量分析。该分析方法也应用于犬血浆中阿利纳斯汀的测定并进行了验证。使用PH柱从加标犬血浆样品中的回收率约为65%。日内和日间精密度分别为7%和12%。犬血浆中的检测限和定量限分别为0.024和0.078μg/ml。
