【作者】 宋丽洁；

【导师】 王唯红； 胡欣；

【作者基本信息】 山东大学 ， 药物分析， 2007， 硕士

【摘要】 中药是我国传统医学的瑰宝，中药中微量元素的研究是中药研究的重要内容。论文建立了微波消解/ICP-MS方法同时测定了大黄、黄芪、黄芩、何首乌、地黄5种中药中的18种元素，对其炮制前后元素的含量及初级形态的变化进行了比较研究，对其中的微量元素与炮制的关系进行了初步的探讨。论文建立了微波消解-电感耦合等离子体质谱法，测定了上述5种中药炮制前后药材中及相应的水煎液中Mg、Al、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Mo、Cd、Sn、Ba、Hg、Pb等18种元素的含量水平。实验对微波消解前处理方法进行了研究，从消解体系、消解液用量、消解程序等几方面对微波消解条件进行了确定，为大黄等根和根茎类中药的消解提供了参考。实验对电感耦合等离子体质谱仪的各项技术参数进行了选择，各项方法学验证证指标，如对18种元素的检出限都在1μg/L以下，精密度在2.39％～8.90％，加样回收率在70％～130％。对5种中药及其炮制品的微量元素测定结果显示中药炮制前后药材中元素含量发生了变化，表明炮制过程对中药中微量元素的总的含量有影响。在测定了5种中药及其炮制品药材中元素含量的基础上，对5种中药及其炮制品进行了元素的初级形态分析。依照初级形态分析流程，制成初级形态分析样品，用微波消解-电感耦合等离子体质谱法测定了其中18种元素的含量，并计算出提取率、残留率、浸留比等形态分析参数。结果表明，不同中药中元素煎出难易顺序不同，同一种中药炮制前后元素的煎出难易顺序也发生了变化，每种中药都有其特有的易于煎出元素，说明每种中药中实际发挥作用的元素不一样。几种中药中Al、V、Cr、Fe等元素残留率均很高，Zn、Mg、Mn等元素的提取率都很高，这可能与它们各自在中药中的存在形态有关。初级形态分析给出了比元素总含量测定更多和更有用的信息。炮制后水煎液中微量元素的含量和提取率的比较中发现黄芪、黄芩、何首乌、地黄4种中药炮制前后水煎液中元素的含量变化与文献中关于药性和微量元素相关性的讨论一致，即：温(热)性药物经炮制后多数元素含量降低，凉(寒)性药物经炮制后多数元素含量升高，微量元素是否与药性变化有关尚需进一步的药理实验证实。炮制后不仅元素含量发生了变化，水煎液中元素的提取率也发生了变化，部分元素提取率发生变化很大，使含量变化发生逆转，提示炮制可能改变了元素的存在形态，使其更易溶出或不易溶出。黄芪、何首乌、地黄3种中药炮制后其中的Mg、Mn、Fe、Zn等补益元素的提取率和含量都有明显升高，而3种中药炮制品均有明显的补益作用，提示微量元素可能与其中的有机成分有协同作用。更多还原

【Abstract】 Chinese traditional medicine is treasure of Chinese traditional physic. The study of trace elements contained in Chinese traditional medicine is an important part of the Chinese traditional medicine research. A method was established for the determination of Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Sn, Ba, Hg and Pb in Radix et rhizoma rhei, radix astragali, radix scutellariae, radix polygoni multiflori and radix rehmanniae by microwave digestion-ICP-MS. The contents and primary speciations of 18 trace elements contained in the five Chinese traditional medicines, their processed products and their respective decoctions were studied. Tentative discussion about the relationship between trace elements and processing, drug properties was made.A method was established for the determination of 18 elements in five Chinese traditional medicines, processed products and their respective decoctions by microwave digestion-ICP-MS. The suitable sample preparation had been developed. The microwave digestion condition was optimized from digestion system, proportion of acids and digestion procedure, which affords reference for the preparation of root and rootstalk herds. Parameters of ICP-MS were optimized. Detection limits of all elements were lower than 1 μg/L, precisions were between 2.39% and 8.90%, recoveries were between 70%-130%. The accuracy was verified by tea standerd reference material. The analytical results of tea SRM were within the certificated values. The result showed that the contents of elements changed before and after processing, implying the procedure of processing had some impact on the contents of elements.Primary speciation of 18 trace elements (Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Sn, Ba, Hg and Pb) was studied. The samples of primary speciation were obtained from primary analytical flow, and the contents of 18 trace elements were determined by ICP-MS. The parameters of species distribution, such as extractive rate, residual rate, immerse-residue ratio etc were also caculated. The elements oder of decoction from difficult to easy in different Chinese traditional medicines was different. It was also differential after and before processing. Each herb had its’ characteristic elements easy to be decocted, indicated that these elements had the greater function. In these herbs, the residual rates of Al, V, Cr, Fe were biger than other elements, the extractive rates of Zn, Mg, Mn were biger than other elements. It showed some relationship to their speciations. More datum and usefull information were gained than gross of elements, because the analysis of primary speciation was gained by traditional decoction. In comparison of contents and extractive rates of trace elements after and before processing, we found that the content diversities caused by processing of radix astragali, radix scutellariae, radix polygoni multiflori and radix rehmanniae were coincident to the relationship between contents and drug properties which had been reported. After processing, the contents of elements in warm (hot) drugs degraded, and the contents of elements in cool (cold) drugs ascensused. The content diversities of radix et rhizoma rhei caused by processing were not coincident to the report. Advanced research was required. Not only the contents but the extractive rates changed. It showed that processing made the speciation of some trace elements change, resulting some elements easy to be decocted or difficult to be decocted.The contents and extractive rates of Mg, Mn, Fe, Zn in radix astragali, radix polygoni multiflori, radix rehmanniae were bigger after processing, it was considered that these herbs had the tonification, and implied the restorative characties of Mg, Mn, Fe, Zn and their organic principles cooperate with each other.更多还原