Study on the Thermal Degradation Behavior of Tanshinones during the Process of Reflux Extraction

用甲醇作提取溶剂,在回流条件下考察了从丹参药材中提取丹参酮类有效成分的过程中,隐丹参酮、丹参酮I及丹参酮IIA等三种丹参酮的热降解行为。结果表明,回流提取过程中所考察的三种丹参酮均发生严重的热降解,降解速率:丹参酮IIA>丹参酮I>隐丹参酮,其热降解均具有零级反应动力学特征;同时,回流提取过程中丹参酮的热降解是在丹参酮共萃物存在下发生的。Thermal degradation behavior of cryptotanshinone,tanshinone I and tanshinone IIA has been studied during the process of reflux extraction of tanshinones from Salvia miltiorrhiza Bge.with methanol as extracting solvent.The obtained results showed that the thermal degradation of cryptotanshinone,tanshinone I and tanshinone IIA occurred obviously during reflux extraction in the order of degradation rate:tanshinone IIA>tanshinone I>cryptotanshinone,and their thermal degradation was featured with zero order reaction;meanwhile,it was under the existence of other components coextracted with tanshinones that the thermal degradation of cryptotanshinone,tanshinone I and tanshinone IIA occurred.国家自然科学基金重点项目(20235020

Ultrasound-assisted Extraction of Tanshinones from Analytical Samples of Salvia miltiorrhiza Bge.

为了提取丹参分析样品中隐丹参酮、丹参酮I及丹参酮IIA等有效成分,建立了以CH3OH-CH2Cl2为提取溶剂的超声波辅助提取法。优化的提取条件是,液/固比:133.3 mL/g,提取溶剂组成:φ(CH2Cl2)=0.2,提取时间:8 min。与几种常规提取法(如甲醇回流法、CH3OH-CH2Cl2室温浸取法)相比较,超声波辅助提取法具有提取时间短、丹参酮提取量高等优点,适用于丹参中隐丹参酮、丹参酮I及丹参酮IIA同时测定的样品前处理。An ultrasound-assisted extraction method for cryptotanshinone,tanshinone I and tanshinone IIA from analytical samples of Salvia miltiorrhiza Bge.was established.The optimal extraction conditions were obtained as follows:φ(CH_2Cl_2)=0.2 CH_3OH-CH_2Cl_2 as extracting solvents,8 min of extraction time and 133.3 mL/g of extracting solvent-to-sample ratio.Compared with conventional methods,such as methanol reflux extraction and CH_3OH-CH_2Cl_2 macerating at room temperature,the method of ultrasound-assisted extraction has the advantages of short extraction time and high efficiency for extracting tanshinones,which suggests that it is suitable for sample pretreatment in the simultaneous determination of cryptotanshinon,tanshinone I and tanshinone IIA in Salvia miltiorrhiza Bge..国家自然科学基金重点项目(20235020

Content and Distribution Characteristics of Anti-oxidant Components from Salvia miliorrhiza Bge

借助超声波萃取法、以反相高效液相色谱 (RP -HPLC -DAD)为分析检测手段 ,研究了丹参 6种抗氧化成分的提取方法和分离定量条件 ,并对这些成分在全株丹参不同部位中的含量分布特征进行了探讨。结果表明 :常温下的超声波萃取可避免热解作用给丹参酮类化合物带来的损失 ,而辅助的加热处理可使原儿茶醛获得较高的提取率 ,两种操作方法简单可行。 6种化学成分在丹参不同部位及不同等级中的分布有较大差异。丹参酮类化合物主要分布在根部皮层 ,而叶子中丹参素的含量却较为丰富 ,可为丹参品质鉴定和质量标准研究及该资源的综合利用奠定理论基础。Extract method and determination parameters for 6 anti-oxidants from Salvia miliorrhiza Beg (Danshen) were reported by means of microwave oven and Reversed-Phase-High-Performance-Liquid-Chromatography (RP-HPLC). These components in different tissue of Danshen were also discussed. The results showed that the loss of tanshinones caused by heating depression could be avoided by means of microwave method at the room temperature, and a higher extraction yield was also obtained by heating. The two extraction methods were simple and easy to operate. The content of tanshinones and salvia acids varied with different tissue and grades. Tanshinones were mainly in cortex of Danshen root, and Danshensu in its leaves. It has great significance for Danshen identification and quality control.香港特别行政区创新科技署创新基金;; 厦门大学现代分析科学教育部重点实验室开放基金共同资

中药质量控制与安全性评价中的分析化学

本文论述了中药现代化实施中进行质量控制的“5P”(GAP、GCP、GLP、GMP、GSP)系统工程 ;结合本实验室近年来以“5P”指导中药质量控制与安全性评价所做的一些工作 ,阐明了将分析化学应用于中药质量控制与安全性评价的策略与方法 ,提出了分析化学在中药现代化系统工程及重大科学问题的解决中所能发挥的重要作用

Determination of Andrographolide and Dehydroandrographolide in Andrographis paniculata Nees Materials and Related Patent Medicines by Reversed-Phase High Performance Liquid Chromatography

发展了穿心莲药材及其中成药中两种主要成分穿心莲内酯和脱水穿心莲内酯的反相高效液相色谱测定方法。采用甲醇振荡提取法进行样品前处理 ,在以乙腈 水为流动相作梯度洗脱、ODS柱、检测波长为 2 2 5nm的条件下 ,穿心莲内酯和脱水穿心莲内酯在 1 5min内可达到基线分离。两种内酯在 1 0mg/L～ 1 0 0mg/L时其浓度与峰面积成良好的线性关系 ,加标回收率为 96 %～ 1 0 4 %。该法适用于穿心莲药材及其制剂的质量分析检验A simple and accurate method for the determination of andrographolide and dehydroandrographolide in andrographis paniculata Nees materials and patent medicines with high performance liquid chromatography (HPLC) has been developed. The two components were extracted from powdered samples by shaking with methanol. The resultant extracts were separated within 15 min on a BECKMAN C 18 column (4 6 mm i d ×250 mm, 5 μm) and with a gradient elution of acetonitrile water at a flow rate of 0 5 mL/min . The detection wavelength was 225 nm and the injection volume was 20 μL. In gradient elution program the volume fraction of acetonitrile in mobile phase was as follows: 0 min-1 min, 40%; 1 min-5 min, 40%-50%; 5 min-15 min, 50%-70%. Both andrographolide and dehydroandrographolide have good linearity in the range of 10 mg/L to 100 mg/L with the correlation coefficients of 0 997?6 and 0 998?6 respectively. This method has been successfully applied for the analysis of andrographis paniculata Nees materials and related patent medicines.科技部中药现代化重中之重项目( 99 92 9 0 213);; 福建省科技部中药质量控制重点项目 (2 0 0 0F0 0 1)

Progress in Analysis of Traditional Chinese Medicines for Organochlorine Pesticide Residues by Gas Chromatography

综述了中草药及其制剂中有机氯类农药残留的气相色谱分析技术,包括样品前处理方法,气相色谱分离分析及确证鉴定技术,对近几年来该领域研究进展进行了总结和讨论。This paper was mainly concerned on the application progress of gas chromatography(GC)in the analysis of Traditional Chinese Medicines(TCMs)for organochlorine pesticide residues(OCPs),such as DDTs and HCHs.The related procedures or techniques for extraction,clean_up,preconcentration,GC separation and identification/confirmation were reviewed respectively.Some typical analytical protoˉcols for several herbal materials(such as Radix Ginseng,Salvia miltiorrhiza Bge.,Herba Asari and etc.)or patent medicines were outlined in table.国家自然科学基金2003重点项目(20235020);; 亿利集团公司甘草GAP项

Continuous Tipless Electrospinning with Rotatory Electrode

连续供液的旋转电极式无针尖静电纺丝采用圆柱滚筒电极代替喷丝头实现了高产量纳米纤维制造.该方法避免了喷丝头的堵塞问题,同时也实现了纳米纤维的连续生产.本文利用扫描电镜(SEM)探讨了该制作过程中的关键参数,如溶液浓度、偏置电压、旋转速度以及溶液厚度等对纳米纤维直径的影响.实验结果表明,纳米纤维的平均直径随溶液浓度、圆柱滚筒电极旋转速度和溶液厚度的增大而增大,但随着偏置电压、圆柱滚筒电极直径的增大而减小.圆柱滚筒电极长度为12 CM、直径为60 MM时制备的纳米纤维产量高达8.7 g/H,且纳米纤维的直径均小于500 nM.Tipless electrospinning with rotatory electrode and continuous supply polymer solution,which uses a cylindrical-shape rotatory electrode to replace syringe spinneret,is a novel method for massive production of nanofibers.It not only avoids the blockage of spinneret but also realizes the continuous production of nanofibers.In this paper,the effects of some key parameters such as solution concentration,applied bias voltage,rotatory speed and thickness of solution on the diameter of nanofibers were discussed via scanning electron microscope( SEM).The results demonstrate that the mean diameter of electrospun nanofibers increases with the increase of solution concentration,rotatory speed of cylindrical-shape rotatory electrode and thickness of solution,but decreases with the increase of applied bias voltage and diameter of cylindrical-shape rotatory electrode.The output of nanofibers achieved 8.7 g / h for a cylindricalshape rotatory electrode( 12 cm in length and 60 mm in diameter),and the diameters of nanofibers were less than 500 nm.supportedbyKeyProgramofNationalNaturalScienceFoundationofChina(51035002);theNationalNaturalScienceFoundationofChina(51205334); theNaturalScienceFoundationofFujianProvinceofChina(2011J05139)~

The applications of analytical techniques in the study on ocean polymetallic nodule and the quality of Chinese medicine

本文针对大洋多金属结核和中药质量研究的需要，运用多种现代分析化学技术，发展了用于这两类复杂基体样品中元素、形态、有效成分或有害物质的分析方法，这些方法均己在具体研究课题中得到应用并取得满意的效果，为从事大洋多金属结核和中药质量方面的相关研究提供了方法学上的基础。本文的主要贡献是：1.发展了大洋多金属结核中27种元素的等离子体质谱(ICP-MS)测定方法。这27种元素包括Ba,Ce,Co,Cu,Dy,Er,Eu,Gd,Ho,La,Li,Lu,Mo,Nd,Pr,Sb,Sc,Sm,Tb,Th,Tm,U,V,W,Y,Yb和Zn。2.建立了中药（人参、丹参）产品中的多种有效成分的分离分析方法。3.提出了...To meet the demands of the study on polymetallic nodule and Traditional ChineseMedicines (TCM), several novel analytical protocols have been proposed usingmodern analytical techniques, such as lCP-MS, GC-ECD/MS, or HPLC-UV/ESIMS.Successful applications of the protocols show that they can provide the relatedresearch projects with the solid base in methodologies. The main contents in thedissertation...学位：博士后院系专业：海洋与环境学院海洋学系_海洋化学学号：BHBG0003

FUNDAMENTAL AND APPLICATION STUDY ON MERCURY SPECIATION WITH GC/MS IN ENVIRONMENTAL AND BIOLOGICAL FIELDS

尽管质谱早已成为气相色谱的一种常规检测器，但气相色谱-质谱联用仪(GC/MS)在元素化学形态分析中的应用却较少。随着质谱灵敏度的不断提高，GC/MS可能成为元素化学形态分析一种有前途的分析技术。本工作的任务是以GC/MS为分离、检测手段，开展环境、生物样品中汞的形态分析研究。 全文由五章组成：1.文献综述：环境、生物样品中汞的形态分析；2.四苯硼钠衍生/溶剂萃取后气相色谱-离子阱质谱测定水中甲基汞；3.超声波辅助萃取法用于水底沉积物中甲基汞的气相色谱-离子阱质谱分析；4.巯基纤维素固相盘萃取、气相色谱-离子阱质谱法测定水、尿中汞形态；5.气相色谱-离子阱质谱分析尿中汞形态。 第一章首先...Presumably owing to its poor sensitivity and high cost relative to atomic absorption spectrometry (AAS) or atomic fluorescence spectrometry (AFS), mass spectrometry (MS) has gained seldom applications in mercury speciation studies. However, the continuous improvements in the sensitivity of MS instrumentation together with its species-selective detectability will probably make it a promising techn...学位：理学博士院系专业：化学化工学院化学系_分析化学学号：B1995220

GC-MS Separation and Identification of Four Mercury Species as Their n-Butyl Derivatives

将无机汞、甲基汞、乙基汞、苯基汞等4种形态汞 ,经葛氏试剂衍生为相应的正丁基衍生物后 ,在弱极性SE -54熔融石英毛细管柱上研究了其衍生物的色谱行为。在优化的色谱条件下 ,4种形态的汞在9min内达到基线分离。此外 ,提供了4种形态汞的正丁基衍生物的电子轰击质谱信息。Four important Hg species in environment, including inorganic, methyl_, ethyl_ and phenyl _ mercury, were derivatized by using n _ butyl Grignard reagent. Under the optimal chromatographic conditions, the resulting derivatives were separated completely on an SE-54 fused silica capillary column within 9 min. In addition, the EI (70 eV) mass spectra of the n _ butyl derivatives of four mecury species are presented.国家自然科学基金!委重点项目(29735160