A micellar enhanced synchronous scanning-dual wavelength fluorimetric method for simultaneous determination of epinephrine,norepinephrine and dopamine has been described.After adding the sensitizing reagent,the ramifications of E,NE and DA have been respectively scanned simultaneously to examine the effect of the micellar enhanced and the factors as pH,the type and dosage of ordered medium(surfactants and cyclodextrin),reaction time,product stability,and so on which affect the intensity of systematic fluorescence.The results showed that when λ_ex was 300.0 nm,Δλ was 70.0 nm,the largest fluorescence signal of DA,which was 385.0 nm,was not disturbed in the simultaneous fluorescence spectrum gained and the mutual interference of E and NE could be eliminated by the dual-wavelength method.The largest fluorescence intensity could be got in 0.3 mol/L acetic acid-sodium acetate buffer at pH 4.6 and the heating time of E,NE and DA were 1 min,2 min and 40 min respectively.The linear ranges were 0.40~32.00 μg/L(r = 0.999 4) for epinephrine,2.45~54.00 μg/L(r = 0.999 5) for norepinephrine and 0.40~45.00 μg/L(r = 0.999 4) for dopamine.The detection limits of E,NE and DA were 0.09,0.27 and 0.08 μg/L respectively.Satisfactory results were obtained by the proposed method for determination of trace amounts of neurotransmitters in several synthetic samples.
目的 通过观察麦冬细胞超声破壁时间和利用紫外分光光度法检测超声提取麦冬皂苷D含量两种考察指标来比较筛选麦冬皂苷D的提取条件,优化超声提取工艺.方法 采用正交设计法,分别以麦冬细胞破壁时间和采用紫外分光光度法测定麦冬细胞破壁后皂苷D的含量为考察指标,考察乙醇浓度、温度、麦冬粒度和先期浸泡时间等因素对超声提取工艺的影响.通过显微镜观察,确定细胞破壁状况;通过对两种考察指标的实验结果 进行比较,优化提取方案.结果 利用紫外分光光度法测定麦冬皂苷D含量和通过观察麦冬细胞破壁所筛选的麦冬皂苷D最佳提取工艺的结果 是一致的.在考察因素中,麦冬皂苷提取工艺影响程度为:粒度﹥乙醇浓度﹥先期浸泡时间﹥温度,超声提取最佳条件为:温度45 ℃,80 目粒度,95% 乙醇,先期浸泡12 h.结论 通过超声方法 对中草药有效成分进行提取,其提取率与细胞破壁有关,利用正交实验分析紫外分光光度法检测麦冬皂苷D含量和考察麦冬细胞破碎的结果 是一致的,可通过观察麦冬细胞破壁结果 来优化提取工艺,简化操作.
胶束毛细管电泳在分离科学中的应用已有广泛报道,但因其检测灵敏度不高,故其在痕量分析中的应用受到一定限制.