【作者】 高静；

【导师】 邓光辉；

【作者基本信息】 广西民族大学 ， 应用化学， 2012， 硕士

【摘要】 迷迭香酸是1958年由Ellis从迷迭香中提取发现的，具有很高的药用价值和美容功效，广泛应用于医药、化妆品及食品等行业，因此对它进行分析研究具有重要意义。由于毛细管电泳紫外检测的灵敏度较低，建立一种测定中药或化妆品中微量迷迭香酸的新方法是有十分必要的。虽然毛细管电泳在测定中药活性成分方面已有一定的应用，但在迷迭香的质量控制方面仍需进行深入研究。此外，有关毛细管电泳对化妆品中迷迭香酸的分析还未见报道。因此，本文根据发展趋势并结合实验室的实际情况，开展了学位论文的研究工作。主要内容如下：1、丹参中迷迭香酸的提取研究本文对丹参中迷迭香酸的提取工艺进行研究。采用超声波提取的方法，在单因素、单水平条件下，对料液比、甲醇浓度、提取温度、提取时间4个因素进行正交设计，以丹参中提取迷迭香酸的含量作为丹参提取的验证指标，用毛细管电泳法对提取物进行定性和定量分析。结果是在料液比为1:25，50%的甲醇在75℃温度下提取30min时，提取效果最好。2、胶束毛细管电泳测定丹参及复方丹参片中迷迭香酸的含量建立胶束毛细管电泳测定丹参及复方丹参片中迷迭香酸的含量。采用重力进样75s，缓冲溶液为25mmol/L硼砂-40mmol/L十二烷基硫酸钠，pH值为9.85，电压为13kV，检测波长为320nm。结果：在上述条件下，迷迭香酸(RA)的线性回归方程式为y=18117x+3157.4(r=0.9968)，线性范围为2.5～100μg/mL，检出限达到0.25μg/mL，迷迭香酸的回收率为92%～105%，RSD为3.2%。结论：该方法简单、准确，可用于丹参及复方丹参片中迷迭香酸的含量测定。3、动态pH联接-扫集毛细管电泳测定化妆品中迷迭香酸的含量采用动态pH联接-扫集毛细管电泳法对化妆品中的迷迭香酸进行检测。采用重力进样的方式，进样高度为15cm的情况下，研究了硼砂浓度、pH值、十二烷基硫酸钠(SDS)浓度、甲醇浓度、样品基体、进样时间、分离电压对富集与分离的影响。优化后的实验条件：15mmol/L硼砂-45mmol/LSDS(pH8.8)-15%甲醇为缓冲液，进样时间60s，分离电压16kV，样品中磷酸盐浓度10mmol/L，样品基质pH为4.7。在上述条件下，迷迭香酸(RA)的线性回归方程式为y=539200x+53588(r=0.9985)，线性范围为0.144~3.6μg/mL，检出限达到0.036μg/mL，迷迭香酸的回收率为92.5%～103%，相对标准偏差(RSD)为2.5%。4、迷迭香的毛细管电泳特征图谱研究建立了迷迭香水溶性成分的毛细管电泳特征图谱。以20mmol/L硼砂(pH=9.50)为背景电解质溶液，运行电压12kV，紫外检测波长300nm，对不同产地迷迭香进行检测。按电泳峰共有率fi≥90%为依据，确定10个不同产地迷迭香的毛细管电泳特征峰为11个，各产地迷迭香的毛细管电泳特征图谱与标准毛细管电泳特征图谱的相似度较好。在制备供试液后不同时间进样测定，各特征峰的相对迁移时间的相对标准偏差小于5.0%，相对峰面积的相对标准偏差在2.7%～8.0%之间，结果表明样品在36h内稳定。该方法简便准确，为迷迭香的质量控制提供了有效的手段。更多还原

【Abstract】 Rosmarinic acid was found from the extracts of rosemary by Ellis in1958. It was used widely in the fields of pharmaceutical, chemical, cosmetics due to its medicinal value and cosmetology effection. Thus, analysis research on rosmarinic acid is of great significance. Because of lower concentration sensitivity of capillary electrophoresis with UV-Visible detection, it is important to propose new methods for the determination of rosmarinic acid in Chinese herbal medicines or cosmetics. Since the application of CE on herbal medicine is already in process, futher investigation should be made to meet the demand for quality control of Rosemary. Besides, there has not seen previous reports on the determination of analytes in cosmetic by CE. Therefore, author chose the subject of dessertation according to the development trends combined with the actual situation of the laboratory in the paper. The main contents of the desertion were as follows:1. Study on extraction of rosemary acid of SalviaExtraction conditions of rosemary acid in Salvia were studied in the paper. Using ultrasonic extraction method, in single factor and level conditions, the orthogonal design condition contain:the ratio of solid liquid, methanol concentration, extraction temperature and extraction time. Qualitative and quantitative analysis of extracted content of rosmarinic acid of Salvia miltiorrhiza was done by method of capillary electrophoresis and used as validation index. Results showed that optimum experimental conditions were:ratio of material liquid1:25,50%methanol, temperature75℃, extraction time30min.2.Determination of rosmarinic acid in salvia miltiorrhiza and compound salvia tablets by micellar electrokinetic capillary electrophoresisA new method based on micellar electrokinetic capillary electrophoresis has been developed for determination of rosmarinic acid in salvia miltiorrhiza and compound salvia miltiorrhiza tablet. Using the inject method of gravity, the sample was injected in75s, the buffer solution was composed of25mmol/L borax-40mmol/L SDS, pH was9.85, the applied voltage was13kV, detection wavelength was set at320nm. Under the optimum conditions, linear equation of RA was y=18117x+3157.4, the correlation was0.9968. The linear range was2.5-100μg/mL and the detection limits was0.25μg/mL. The recovery found were in the range from92%to105%, with RSD of3.2%.The method is simple and accurate. It can be used to detect rosmarinic acid in salvia miltiorrhiza and compound salvia tablets.3.Determination of rosmarinic acid in cosmetics by Dynamic pH Junction-sweeping in capillary electrophoresisA method of dynamic pH junction-sweeping in capillary electrophoresis was achieved for the analysis of rosmarinic acid in cosmetics. In the case of the sample height is15cm by gravity sampling, the study of some conditions which are the concentration of borax, pH value, the concentration of SDS, the concentration of methanol, sample matrix, sampling time, separation voltage were optimized. The optimized experimental condition:the buffer:15mmol/Lborax-45mmol/L SDS(pH8.8)-15%methanol, the sampling time was60s, the applied voltage was16kV, the concentration of phosphate in the sample was10mmol/L. The pH of sample matrix was4.7.The linear equation of RA was y=539200x+53588, the correlation was0.9985.The linear range was0.144-3.6μg/mL and the detection limits was0.036μg/mL. The recovery found was in the range from92.5%to103%, with RSD of2.5%.4.Study on Capillary Electrophoresis specific chromatogram of rosmarinus officinalisThe electrophoretic specific chromatogram of water-soluble constituents of rsomarinus officinalis was established by capillary electrophoresis.20mmol/L borax (pH=9.50) was used as background electrolyte, and running voltage of12kV was applied. UV-detection at the wavelength of300nm was adopted. Samples of rosmarinus officinalis in10different areas were taken for analysis. Base on the value of rate of common elect rophoretic peaks fi≥90%, a set of electrophoretic characteristic atlas of11peaks was determined for flavones in rsomarinus officinalis samples from10different areas. Good similarities between the electrophoretic finger print atlases of the samples and the standards were obtained. Relative standard deviation among the values of relative migration times of various specific peaks obtained at different time of sample introduction was less than5.0%, and values of RSD for the relative peak areas were in the range from2.7%to8.0%. The results obtained proved that the sample was stable within36h. The method is simple, accurate and suitable for the quality control of rosmarinus officinalis.更多还原