Palumbo G, Carlucci G, Mazzeo P, Frieri G, Pimpo M T, Fanini D
Department of Internal Medicine, University of L'Aquila, Italy.
J Pharm Biomed Anal. 1995 Dec;14(1-2):175-80. doi: 10.1016/0731-7085(95)01608-2.
A high-performance liquid chromatographic method for the simultaneous determination of 5-aminosalicylic acid (5-ASA), acetyl-5-aminosalicylic acid (Ac-5-ASA) and 2,5-dihydroxybenzoic acid (5-HSA) in human endoscopic intestinal biopsy with electrochemical detection has been developed and validated. A liquid-liquid extraction procedure was used to isolate these drugs from the biological material prior to analysis. The compounds were separated on an Erbasil S reversed-phase column using methanol-critic acid-sodium hydrogenphosphate-heptane-sulfonic acid-disodium ethylenediaminetetraacetate (pH 3) as mobile phase. The method was linear from 1.0 to 300 ng ml-1 for 5-ASA, from 10 to 1000 ng ml-1 for Ac-5ASA and from 0.1 to 10 ng m-1 for 5-HSA. The limit of detection for 5-ASA and for Ac-5-ASA was 1 ng ml-1 and that for 5-HSA was 0.1 ng ml-1. This procedure is suitable for pharmacological and clinical studies of 5-ASA.
已开发并验证了一种高效液相色谱法，用于在电化学检测下同时测定人内镜肠道活检组织中的5-氨基水杨酸（5-ASA）、乙酰-5-氨基水杨酸（Ac-5-ASA）和2,5-二羟基苯甲酸（5-HSA）。在分析之前，采用液-液萃取程序从生物材料中分离出这些药物。使用甲醇-柠檬酸-磷酸氢二钠-庚烷-磺酸-乙二胺四乙酸二钠（pH 3）作为流动相，在Erbasil S反相柱上分离这些化合物。该方法对于5-ASA在1.0至300 ng/ml范围内呈线性，对于Ac-5ASA在10至1000 ng/ml范围内呈线性，对于5-HSA在0.1至10 ng/ml范围内呈线性。5-ASA和Ac-5-ASA的检测限为1 ng/ml，5-HSA的检测限为0.1 ng/ml。该程序适用于5-ASA的药理和临床研究。
