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近年来,巴氯芬(Baclofen,对氯苯基-γ-氨基丁酸)广泛用于治疗肌痉挛。已知测定方法有气相法、质谱法和荧光法。本文报道一种快速、灵敏的分光光度法,其原理为巴氯芬与试剂2,4,6-三硝基苯磺酸(TNBS)于碱性介质中能生成一种稳定的黄色衍生物,最大吸收波长为358nm,可用于制剂的分析。对反应的pH、温度和试剂的用量进行试验的结果表明,选择最佳条件为:pH=11,试剂与药物的分子比为7,于室温30min 时能达到最大吸收,并能稳定30~40min。溶液在2~14μg/ml 范围内,吸收度与浓度呈线性关系(γ=0.99991);同一溶液(8μg/ml)10次测定的变异系数为0.07%.此法可用于巴氯芬片的测定,与茚三酮法得到的结果相比,其平均值与标准差无显著差异,平均回收率分别为95.3±0.08%与95.4±0.09%。标准曲线的制备:精密秤定巴氯芬约20mg,置50ml 容量瓶中,加蒸馏水至刻度,摇匀,精密量取由25~175μl(每份25μl)溶液分别置5ml 容量瓶中,各加新鲜
In recent years, baclofen (p-chlorophenyl-γ-aminobutyric acid) has been widely used to treat muscle spasms. Known determination methods are gas phase method, mass spectrometry and fluorescence method. This paper reports a fast and sensitive spectrophotometric method based on the principle that baclofen and reagent 2,4,6-trinitrobenzene sulfonic acid (TNBS) can form a stable yellow derivative in alkaline medium, The maximum absorption wavelength of 358nm, can be used for the analysis of the preparation. The results of the reaction pH, temperature and the amount of reagent showed that the optimum conditions were as follows: pH = 11, molecular ratio of reagent to drug 7, maximum absorption at room temperature 30min and stable 30 ~ 40min . The concentration of the solution was linear in the range of 2-14 μg / ml (γ = 0.99991), and the coefficient of variation (CV) was 10% in the same solution (8 μg / ml) for 10 times.The method was applied to the determination of baclofen tablets Compared with the ninhydrin method, the mean and standard deviation of the two methods were not significantly different. The average recoveries were 95.3 ± 0.08% and 95.4 ± 0.09%, respectively. Preparation of the standard curve: Precision scale set baclofen about 20mg, set 50ml volumetric flask, add distilled water to the mark, shake, the precise amount of 25 ~ 175μl (25μl each) solution were set 5ml volumetric flask, plus fresh