Tosunoğlu S, Ersoy L
Faculty of Pharmacy, Department of Analytical Chemistry, University of Istanbul, Turkey.
Analyst. 1995 Feb;120(2):373-5. doi: 10.1039/an9952000373.
An isocratic reversed-phase column liquid chromatographic assay for baclofen was developed. Prior to analysis, derivatization of urine or deproteinized plasma with 4-chloro-7-nitrobenzofurazan (NBD-CI) reagent was employed. After solid-phase extraction on a small silica gel column, the mixture was chromatographed on a 10 microns Bondapak C18 column using methanol-water (45 + 55 v/v) as the mobile phase. The NBD-baclofen derivative was detected spectrofluorimetrically by monitoring the emission at 524 nm with excitation at 463 nm. The method was tested for suitability in routine analysis. After a single oral dose of 20 mg of baclofen, the plasma concentration and the cumulative urinary excretion of the drug were determined. The average recoveries were 99.5 and 98.5% for plasma and urine, respectively.
建立了一种用于巴氯芬的等度反相柱液相色谱测定法。在分析前,用4-氯-7-硝基苯并呋咱(NBD-CI)试剂对尿液或脱蛋白血浆进行衍生化处理。在小硅胶柱上进行固相萃取后,混合物在10微米的Bondapak C18柱上进行色谱分析,以甲醇-水(45 + 55 v/v)作为流动相。通过在463 nm激发波长下监测524 nm处的发射光,用荧光分光光度法检测NBD-巴氯芬衍生物。对该方法在常规分析中的适用性进行了测试。单次口服20 mg巴氯芬后,测定了药物的血浆浓度和累积尿排泄量。血浆和尿液的平均回收率分别为99.5%和98.5%。