Analysis of Lipid-solubles of Danshen by LC-MS and the Study of the Metabolic and Interaction Behavior

丹参,又称血参、紫丹参、红丹参等,为唇形科鼠尾草属植物丹参(SalviamiltiorrhizaBunge)的干燥根及根茎。始载于《神农本草经》，被列为上品，历代本草均有收载。丹参归心、肝经，药性微寒，味苦、无毒，具有祛瘀止痛、活血调经、养心除烦的功效。丹参在临床上广泛用于治疗心血管系统疾病，具有扩张冠状动脉、增加冠脉血流量、防止心肌缺血和心肌梗塞、改善微循环、降低心肌耗氧量等作用。其有效成分有水溶性和脂溶性两大类，水溶性部分主要为酚酸类化合物(包括丹参素、原儿茶醛、丹酚酸等)；脂溶性部分主要为二萜醌类化合物(包括丹参酮IIA、隐丹参酮等)。 长期以来人们对丹参的研究多集中在其临床药效以及配...Danshen, the rhizome of Salvia miltiorrhiza Bunge, is one of the most important ancient Chinese herbal drugs. It was recorded originally in Shen-Nung’s Pen-Ts’ao，the classic ancient Pharmacopoeia of China, and ranked as a ‘‘Supergrade’’ medicine by the manuscript. Because of its reported biopharmaceutical properties of improving microcirculation, causing coronary vasodilatation, suppressing heart ...学位：哲学博士院系专业：化学化工学院化学系_分析化学学号：B20032501

Analysis of Diterpene Quinones in Danshen(Salvia Miltiorrhiza Bunge) by HPLC-ESI/TOFMS

采用高效液相色谱-电喷雾飞行时间质谱(HPLC-ESI/TOFMS)联用技术,研究4种丹参酮的分子结构与裂解规律间的关系,并对丹参酮中的脂溶性成分进行鉴定。采用反相C18色谱柱,以甲醇-0.1%乙酸+5mmol.L-1乙酸铵溶液为流动相,二元等度洗脱。通过与电喷雾飞行时间质谱联用,获得丹参中脂溶性成分的精确相对分子质量和分子式,采用质谱碰撞诱导解离技术获得各化合物碎片的裂解信息,并对丹参中的16种丹参酮类化合物进行了初步鉴定。研究结果表明,高效液相色谱-电喷雾飞行时间质谱联用技术能够简便、快速、有效地鉴别丹参中的丹参酮类化合物。The diterpene quinone components in lipid soluble fractions of Danshen were studied by HPLC-ESI/TOFMS.The lipid solubles were extracted with a mixture of chloroform and methanol(1∶4,V/V).The extract was dried by a gentle stream of nitrogen,and the residue was diluted in methanol for analysis.HPLC was performed on a reversed-phase C18 column using isocratic elution with a mixture of methanol and water with the addition of 0.1% acetic acid and 5 mmol·L-1 ammonium acetate.Accurate molecular weights of individual tanshinones were determined through ESI-TOF/MS on-line detection.The molecular formula and TOFMS fragmentation behavior of each compound were obtained through off-line analysis under different collision induced dissociation(CID) energies.Combining literature information with the observed data,16 tanshinones in lipid-soluble fractions of Danshen were tentatively identified in a run.The method demonstrates high potential as a rapid and effective method for the preliminary structural screening and speciation of bioactive tanshinone components in Danshen or other herbal extracts.国家自然科学基金“面上项目”(20675021);; 青岛共建生物医药研发测试中心项目(LS-05-KJZX-76)资

Primary Identification of Triterpene Compounds in Chizhi (Ganoderma lucidum) by HPLC-APCI-MS

采用反相高效液相色谱-二极管阵列检测器(RP-HPLC-DAD)和大气压化学电离质谱(APCI-MS)联用技术,分析赤芝中含有的三萜类化合物。使用反相C18色谱柱,以乙腈和水(含2%冰醋酸)为流动相梯度洗脱,流速为0.8ml/min,室温下,色谱检测波长253nm;用DAD检测器记录各个色谱峰的紫外吸收光谱,采用APCI-MS进行在线同步分析,记录TIC总离子流色谱图和各个色谱峰的质谱图,通过紫外光谱及质谱分析并与文献对照初步鉴定了赤芝中的32个三萜类成分。High performance liquid chromatography (HPLC)-atmospheric pressure chemical ionization-mass spectrometry (APCI-MS) was applied to analyze the triterpenoids in extracts of Ganoderma lucidum. The extraction conditions are: Hypersil C4 (4.6 mm × 150 mm) column with gradient elution with acetonitrile and water (2.0% acetic acid) as mobile phase, flow-rate 0.8 ml/min, and room temperature about 25 ℃. The detection wavelength is 253 nm and the UV spectra of peaks are obtainedwith a photodiode array detector (DAD). On-line APCI-MS in positive and negative mode was used to get the mass spectrum of the analyte. Thirty-two components of Ganoderma lucidum are primarily identified by comparison of the UV spectra and mass spectrum according to published literatures.青岛“2004将才计划”项目(04-3-JJ-11);; 共建生物医药研发测试中心资助项目(LS-05-KJZX-76

Y型聚乙二醇干扰素琢-2b注射液治疗HCV基因2/3型慢性丙型肝炎患者疗效和安全性的多中心随机对照试验研究

目的以标准剂量的聚乙二醇干扰素(Peg IFN)α-2a联合利巴韦林作为阳性对照,评价新型试验药物Y型Peg IFNα-2b注射液联合利巴韦林治疗2型/3型慢性丙型肝炎(CHC)患者的疗效和安全性。方法采用多中心、随机开放、阳性药对照的Ⅲ期临床试验,筛选符合要求的2型/3型CHC患者,按照2:1的比例随机分配到Y型Peg IFNα-2b组和Peg IFNα-2a组,同时口服利巴韦林,疗程24 w,停药随访24 w。采用Abbott Real Time HCV Genotype II检测HCV基因型,采用Cobas Taq Man实时定量PCR法检测血清HCV RNA水平。详细记录不良事件。主要疗效指标为持续病毒学应答(SVR),并进行非劣效检验。结果本试验实际入组2型/3型CHC患者255例,实际治疗241例。全分析集(FAS)数据显示,158例试验组和83例对照组患者SVR分别为85.4%(95%CI 79.94%~90.94%)和79.5%(95%CI 70.84%~88.20%,P=0.2402);对符合方案分析集(PPS)人群分析显示,试验组和对照组患者SVR分别为87.9%(95%CI 82.45%~93.27%)和85.9%(95%CI 77.82%~94.01%,P=0.7060),率差的95%可置信区间均符合非劣效标准;对PPS人群分析显示,85.8%受试者获得了早期病毒学应答(RVR),RVR的阳性预测值为90.1%;试验组和对照组不良事件发生率相似,分别为95.6%和95.2%,严重不良事件发生率分别为3.8%和3.6%。结论应用Peg IFNα联合利巴韦林治疗2型/3型CHC患者,新型试验药物Y型Peg IFNα-2b具有与对照药物Peg IFNα-2a相似的疗效和安全性。国家科技部“十二五”重大专项(编号:2012ZX10002-003)；“重大新药创制”十二五科技重大专项(编号:2012ZX09303019)

精细化管理模式在高校后勤管理中的应用分析

目前，高校管理呈现出严谨化、专业化的发展趋势，在高校后勤管理过程中，管理部门需要实施精细化管理模式，节省更多的管理成本，营造良好的校园环境。高校后勤管理部门在应用精细化管理模式的过程中，需要严格按照专业化标准进行管理，深入分析学校个体情况，提高管理效率，论文主要对精细化管理模式在高校后勤管理中的应用进行了分析。</jats:p

高校后勤社会化管理问题及改善策略

在社会改革进程日益推进的大背景下，很多高校还未认识到社会化改革的重要性，高校后勤社会化管理问题日益突显出来，如后勤队伍综合素质参差不齐、产权问题不明确等，这就需要高校后勤管理部门进行全面改革，进一步优化后勤管理体系。论文主要对高校后勤社会化管理问题及改善策略进行了研究。</jats:p

Application of Macroporous Resins in Separating Licorice Flavonoids and Glycyrrhizic Acid

本文在比较了四种大孔树脂对甘草酸和甘草总黄酮静态分离性能的基础上,筛选出大孔树脂XDA-1,对它的动态吸附分离条件如上样液浓度、洗脱溶剂及洗脱流速进行了进一步的研究。结果表明,树脂XDA-1对甘草总黄酮和甘草酸的吸附量大,易于洗脱,分离效果好,最终的黄酮收集液中不含甘草酸。本实验的优化条件为:上样液pH=5,甘草酸浓度为1.5 mg／mL,总黄酮浓度为0.75 mg／mL,上样流速为3 BV／h;洗脱液采用1.5 BV／h 45％的乙醇为最佳。再用含1％NaOH的80％乙醇以1.5 BV／h流速洗脱,得到甘草酸。总黄酮的收率为69.7％,甘草酸收率为52％,纯度为65.5％。Glycyrrhizic acid (GA) and licorice flavonoids (LF) are main bioactive components in licorice. However, long-term excessive intake of glycyrrhizic acid could cause side effect such as sodium retention and hypertension. In order to separate these components individually, and to produce licorice extracts aiming at different applications, a preparative scale separation technique is needed. Against this background, the sorption and desorption properties of licorice flavonoids (LF) and glycyrrhizic acid (GA) on macroporous resins including XDA-1, LSA-10, D101 and LSA-20 have been studied to gain better understandings on the separation characteristics of these resins. The adsorption capability of the resins is found to be strongly dependent on the pH value of the feed solution. Adsorption isotherms were obtained by batch experiments and the data are fitted to the Freundlich equation to evaluate the adsorption properties of these resins. XDA-1 is found to provide the best fit to the Freundlich isotherm. It has much higher adsorption capacity for GA and LF than other resins. XDA-1 shows a higher adsorption affinity towards LF than that of GA based on the calculated adsorption isotherms. Dynamic adsorption and desorption on the selected XDA-1 resin were carried out in a laboratory packed column (0. 5 cm×30 cm) to obtain optimal parameters for LC separation. A simple preparative separation procedure for LF and GA from licorice root was established. An LF enriched extract containing up to 60% LF but without GA contamination; and a GA extract with 65. 6% chromatographic purity have been prepared by the method

一种装配式新型张力计的研制

土体干湿过程引发的岩土工程问题已逐渐受到重视。通常采用张力计量测80 kPa以内的土体吸力,并将其应用于边坡失稳等岩土工程问题的分析中。然而,传统张力计由于内部腔体体积过大且结构复杂,造成张力计难以饱和,吸力量测时反应时间长,并易发生汽化,严重影响其可靠性和灵敏性。为弥补传统张力计的设计缺陷,提出了一种装配式新型张力计。该张力计内腔结构简单且体积小。饱和前先拆分张力计再分别饱和其主要部件,最后重新装配。此设计简化了饱和程序并提高了效率。通过对比传统张力计和新型张力计的性能,证实了新型张力计具有更强的汽化持久性,其吸力量测的灵敏性和可靠性得到了显著的提高。标定试验表明,相比于传统张力计,新型张力计的灵敏性提高了90%。测量-80 kPa的孔隙水压力时,新型张力计的平衡时间为1.5 min,仅占传统张力计反应时间的10%。相同的测量条件下,传统张力计的测量误差为30%,而新型张力计的测量误差仅为0.7%。 Ever more attention has been paid to geotechnical problems induced by wetting and drying of soils recently. Suction up to 80 kPa, measured by tensometers, has been used for analyzing geotechnical problems such as slope instability during wetting and drying. However, existing tensometer generally has a long response time and is easy to cavitate since it has a large volume of water reservoir and complicated internal structure. These drawbacks affect the sensitivity and reliability of a conventional tensometer seriously. In order to overcome these shortcomings, a newly developed fabricated tensometer is introduced. This type of new tensometer with fabricated structure has a simple internal structure and a small volume of water reservoir. At the same time, a drainage hole is introduced to prevent large excess pore water pressure during the process of reassembling. More importantly, its saturation procedure is simple and efficient since the high air-entry ceramic disc and pore pressure transducer of this new tensometer can be disassembled for saturation separately and effectively. After the saturation of the high air-entry ceramic disc and pore pressure transducer, these key components are reassembled together as a tensometer ready for use. As compared with a conventional tensometer, the sensitivity and reliability of this new tensometer are justified. The results of calibration test show that the sensitivity of the new tensometer increases by 90% by comparing with the conventional tensometer. In the case of measuring the pore water pressure of -80 kPa, the equilibrium time required for this new tensometer is only 1.5 minite, about 10% of that for the conventional tensiometer. Moreover, the reliability of the new tensometer is better than that of the conventional tensometer. The measurement error of the conventional tensiometer is about 30%, when measuring the pore water pressure of -80 kPa. Subjected to the same conditions, the new tensometer shows a measurement error of only 0.7%