采用柱后荧光衍生化法建立生物样品中雷尼替丁及其代谢物的液相色谱分析方法。
Use of post-column fluorescence derivatization to develop a liquid chromatographic assay for ranitidine and its metabolites in biological fluids.
作者信息
Viñas P, Campillo N, López-Erroz C, Hernández-Córdoba M
机构信息
Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, Spain.
出版信息
J Chromatogr B Biomed Sci Appl. 1997 Jun 6;693(2):443-9. doi: 10.1016/s0378-4347(97)00075-3.
Ranitidine and its main metabolites, ranitidine N-oxide and ranitidine S-oxide, were determined in plasma and urine after separation using reversed-phase liquid chromatography. The mobile phase consisted of an initial isocratic step with 7:93 (v/v) acetonitrile-7.5 mM phosphate buffer (pH 6) for 8 min, followed by a linear gradient up to a 25:75 (v/v) mixture over 1 min. Detection was carried out by a post-column fluorimetric derivatization based on the reaction of the drugs with sodium hypochlorite, giving rise to primary amines that reacted with o-phthalaldehyde and 2-mercaptoethanol to form highly fluorescent products. The calibration graphs, based on peak area, were linear in the range 0.1-4 microg/ml for all drugs. The detection limits were 30, 41 and 32 ng/ml (8.6, 12.5 and 9.1 pmol) for ranitidine S-oxide, ranitidine N-oxide and ranitidine, respectively. Chromatographic profiles obtained for plasma and urine samples showed no interference from endogenous compounds.
采用反相液相色谱分离后，测定了血浆和尿液中的雷尼替丁及其主要代谢产物雷尼替丁N -氧化物和雷尼替丁S -氧化物。流动相初始为等度洗脱，采用7:93（v/v）乙腈 - 7.5 mM磷酸盐缓冲液（pH 6），持续8分钟，随后在1分钟内线性梯度至25:75（v/v）混合液。通过柱后荧光衍生化进行检测，该衍生化基于药物与次氯酸钠的反应，生成与邻苯二甲醛和2 -巯基乙醇反应形成高荧光产物的伯胺。基于峰面积的校准曲线在所有药物的0.1 - 4 μg/ml范围内呈线性。雷尼替丁S -氧化物、雷尼替丁N -氧化物和雷尼替丁的检测限分别为30、41和32 ng/ml（8.6、12.5和9.1 pmol）。血浆和尿液样本获得的色谱图显示无内源性化合物干扰。
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