Igarashi K, Castagnoli N
Department of Chemistry, Virginia Polytechnic Institute and State University, Blacksburg 24061.
J Chromatogr. 1992 Sep 2;579(2):277-83. doi: 10.1016/0378-4347(92)80392-4.
A sensitive and selective method for the determination of the pyridinium metabolite (HPP+) derived from the antipsychotic drug haloperidol (HP) in brain tissue, plasma and urine using high-performance liquid chromatography with fluorescence detection is described. The HPP+ present in biological samples was extracted using a Sep-Pak C18 cartridge. Recoveries of HPP+ ranged from 78 to 90%. Final separation and quantitative estimations of HPP+ were achieved on a C18 reversed-phase column employing a mobile phase of acetonitrile-30 mM ammonium acetate (40:60, v/v) containing 10 mM triethylamine and adjusted to pH 3 with trifluoroacetic acid. The fluorescence detection utilized an excitation wavelength of 304 nm and an emission wavelength of 374 nm. Standard curves were linear in the range of 2.5-100 ng/ml for brain tissue homogenate and plasma samples and 10-500 ng/ml for urine samples. The detection limit of HPP+ was about 1 ng/ml in all biological samples. The concentrations of HPP+ in brain tissue, plasma and urine from HP-treated rats were determined using this method.
描述了一种灵敏且具有选择性的方法,该方法采用带荧光检测的高效液相色谱法,用于测定脑组织、血浆和尿液中抗精神病药物氟哌啶醇(HP)衍生的吡啶鎓代谢物(HPP⁺)。使用Sep - Pak C18柱提取生物样品中存在的HPP⁺。HPP⁺的回收率在78%至90%之间。在C18反相柱上进行HPP⁺的最终分离和定量测定,流动相为乙腈 - 30 mM乙酸铵(40:60,v/v),含有10 mM三乙胺,并用三氟乙酸调节至pH 3。荧光检测采用304 nm的激发波长和374 nm的发射波长。脑组织匀浆和血浆样品的标准曲线在2.5 - 100 ng/ml范围内呈线性,尿液样品在10 - 500 ng/ml范围内呈线性。所有生物样品中HPP⁺的检测限约为1 ng/ml。使用该方法测定了经HP处理的大鼠脑组织、血浆和尿液中HPP⁺的浓度。