HPLC法测定灯盏花素胶囊中野黄芩苷的含量

建立了灯盏花素胶囊中野黄芩苷的含量的测定方法。采用HPLC测定胶囊中野黄芩苷的含量,C18色谱柱(4.6 mm×250 mm,5μm),柱温40℃,进样量20 uL,流动相:甲醇-0.1%磷酸(40∶60),流速1.0 mL/min,检测波长:335 nm。野黄芩苷在20～160μg/mL范围内,进样量与峰面积积分值之间线性关系良好,平均回收率为99.1%,RSD为0.46%。本方法操作快速简单,准确可靠,可用于灯盏花素片的含量测定和质量控制。     

一种制备野黄芩苷的简单方法

研究灯盏花粗提物中野黄芩苷的制备工艺。通过酸沉法,从灯盏花粗提物中分离得到总黄酮沉淀物,以甲醇为溶剂进行结晶,得到野黄芩苷。结果表明,灯盏花粗提物酸沉pH为1.5,灯盏花总黄酮得率为3.27%,经高效液相色谱检测,所得一次、二次沉淀中野黄芩苷含量分别为92.0%和87.9%,甲醇结晶得到的野黄芩苷含量为94.7%。     

四乙酰乙胺的合成

四乙酰乙二胺,即ＴＡＥＤ是一种低温型漂白活化剂,本实验以乙二胺、冰乙酸、乙权酐为原料,在同一反应釜内,采用两步法合成四乙酰乙二胺。探讨了产品合成工艺条件,产品产这７５．９％。     

四乙酰乙二胺的合成研究

以乙二胺、乙酸、乙酸酐为原料,在同一反应釜内,采用两步法合成四乙酰乙二胺。结果表明,当ｎ（乙二胺）∶ｎ（乙酸）∶ｎ（乙酸酐）＝１∶２５∶４,反应温度为１２０℃（第一步）和１４０℃（第二步）,反应时间为９～１０ｈ时,产品产率可达７５％。     

漂白活化剂四乙酰乙二胺的合成

四乙酰乙二胺(TAED)是一种含氧漂白活化剂,广泛应用于日用化工行业。本课题开发出了两步法合成TAED的工艺路线。第一步以乙二胺、乙酸合成二乙酰乙二胺(DAED);第二步以上述合成液与乙酸酐进一步合成TAED。通过催化剂、原料配比、反应时间、反应精馏等多种因素对TAED合成过程的影响作了考察,从而获得了较佳的工艺条件。     

合成四乙酰核糖的新工艺

以肌苷为原料 ,经酰化 ,合成四乙酰核糖 ,收率为 86 %。     

漂白活化剂四乙酰乙二胺的制备

以乙二胺、乙酸和乙酸酐为原料，采用两步同釜连续制备工艺，制备漂白活化剂四乙酰乙二胺（ＴＡＥＤ），产率达７５％。     

合成反应与精馏过程耦合制备四乙酰乙二胺

采用精馏过程与合成反应耦合技术生产四乙酰乙二胺 ,并研究了物料比、反应温度和时间对产率的影响。结果显示最佳工艺条件为 :n(乙二胺 )∶n(乙酸 )∶n(乙酐 ) =1∶2 .5∶6 ,第一步在 1 2 0℃下反应 3h ,第二步在 1 4 0℃下反应 6h。控制合适的精馏回流比 ,总收率可达 79%。     

漂白活化剂四乙酰乙二胺的制备

本文论述了以乙二胺、乙酸和乙酸酐为原料，采用两步同釜连续制备工艺，分别在１２０℃和１４０℃温度下，制备漂白活化剂四乙酰乙二胺（ＴＡＥＤ）的方法     

Synthesis and bio-activity evaluation of scutellarein as a potent agent for the therapy of ischemic cerebrovascular disease

Scutellarein, the main metabolite of scutellarin in vivo, has relatively better solubility, bioavailability and bio-activity than scutellarin. However, it is very difficult to obtain scutellarein in nature compared with scutellarin. Therefore, the present study focused on establishing an efficient route for the synthesis of scutellarein by hydrolyzing scutellarin. The in vitro antioxidant activities of scutellarein were evaluated by measuring its scavenging capacities toward DPPH, ABTS^+•, ^•OH free radicals and its protective effect on H₂O₂-induced cytotoxicity in PC12 cells using MTT assay method. The results showed that essential point to the synthesis was the implementation of H₂SO₄ in 90% ethanol in N₂ atmosphere; scutellarein had stronger antioxidant activity than scutellarin. The results have laid the foundation for further research and the development of scutellarein as a promising candidate for ischemic cerebrovascular disease.     

A New and Practical Synthetic Method for the Synthesis of 6-O-Methyl-scutellarein: One Metabolite of Scutellarin in Vivo

Scutellarin (1) has been used for the treatment of angina pectoris, cerebral infarction and coronary heart disease with a large market share in China. Pharmacokinetic studies on scutellarin showed that scutellarin (1) is readily converted into its metabolites in vivo. In this paper, a new and practical synthetic method for the synthesis of 6-O-methyl-scutellarein (3) (one metabolite of scutellarin in vivo) is reported. The benzyl bromide was firstly used to selectively replace the acetyl group at C-7 in 7, and was then used to protect the hydroxy groups at C-4'' in 10, 6-O-methyl-scutellarein (3) is obtained in high yield through these methods.     

Pilot-Scale Multi-Stage Countercurrent Extraction of Scutellarein from Erigeron breviscapus (Vant.) Hand-Mazz

Abstract

A low-temperature, timesaving, lower solvent consumption, and energy cost and multi-stage countercurrent extraction (MCCE) technique was developed for pilot-scale production of scutellarein from Erigeron breviscapus (Vant.) Hand-Mazz. The optimum conditions of MCCE process were obtained using the orthogonal array design method, i.e., 70% (v/v) of ethanol water solution, 16 L/kg of solvent to herbal sample ratio, 45°C of extraction temperature and 30 min of extraction time. A comparison between the MCCE technique and single pot extraction (SPE) under respective optimized operation conditions was made and time courses of scutellarein of MCCE and SPE processes were plotted, indicating that the MCCE technique can lower the extraction temperature and decrease five-sixth of the extraction time and two-thirds of the solvent consumption at the equivalent extraction yield of scutellarein.     

香豆素类葡萄糖酯与糖苷化合物的合成与表征

根据3种香豆素衍生物的结构特点,对香豆素类化合物的合成和葡萄糖的Kenigs-Knorr反应进行了研究,采用两种方法,制得3种具有β-构型的香豆素葡萄糖酯及糖苷化合物,并应用核磁共振、红外光谱、元素分析进行了结构表征。     

二茂铁羧酸四乙酰葡萄糖基酯的合成

采用ＰＴＣ法合成了３个二茂铁羧酸四乙酰葡萄糖基酯,通过ＥＡ,ＩＲ,＾ＨＮＭＲ及ＭＳ确证了所合成化合物的结构。     

Inhibition of Cell Proliferation and Metastasis by Scutellarein Regulating PI3K/Akt/NF-κB Signaling through PTEN Activation in Hepatocellular Carcinoma

Scutellarein (SCU) is a well-known flavone with a broad range of biological activities against several cancers. Human hepatocellular carcinoma (HCC) is major cancer type due to its poor prognosis even after treatment with chemotherapeutic drugs, which causes a variety of side effects in patients. Therefore, efforts have been made to develop effective biomarkers in the treatment of HCC in order to improve therapeutic outcomes using natural based agents. The current study used SCU as a treatment approach against HCC using the HepG2 cell line. Based on the cell viability assessment up to a 200 μM concentration of SCU, three low-toxic concentrations of (25, 50, and 100) μM were adopted for further investigation. SCU induced cell cycle arrest at the G2/M phase and inhibited cell migration and proliferation in HepG2 cells in a dose-dependent manner. Furthermore, increased PTEN expression by SCU led to the subsequent downregulation of PI3K/Akt/NF-κB signaling pathway related proteins. In addition, SCU regulated the metastasis with EMT and migration-related proteins in HepG2 cells. In summary, SCU inhibits cell proliferation and metastasis in HepG2 cells through PI3K/Akt/NF-κB signaling by upregulation of PTEN, suggesting that SCU might be used as a potential agent for HCC therapy.     

灯盏花素的提取与分离工艺优化研究

以灯盏乙素的提取率为指标,采用高效液相色谱法对灯盏乙素的含量进行测定,对灯盏花中灯盏花素的提取方法及工艺条件进行了优化.确定较优提取方法为超声波提取法,通过正交实验确定超声波提取法的最优工艺为:以10倍量的70%乙醇提取3次,每次60 min.此时,所得浸膏中灯盏乙素含量达到2.15%,提取率达到83.39%.超声波提取法是一种快速、简便、高效且稳定可行的灯盏花素提取方法.     

灯盏花乙素苷元的制备研究进展

综述了标题化合物的制备方法及最新研究进展。其中,植物提取方法主要是从灯盏花或野黄芩药材中提取分离得到。化学合成方法有全合成和半合成方法,全合成方法以5,6,7,4'-四甲氧基黄酮为起始原料,采用不同的脱甲基试剂合成标题化合物;半合成方法是用灯盏花乙素经水解断糖苷键合成标题化合物。     

多壁碳纳米管修饰玻碳电极测定药物野黄芩苷

采用超声波处理多壁碳纳米管,配成修饰液后滴涂于玻碳电极表面制作成多壁碳纳米管修饰玻碳电极（MWNTs/GCE）。以循环伏安法研究了野黄芩苷在修饰电极上的电化学行为,建立了一种电化学检测野黄芩苷的新方法。结果表明,在最佳条件下,野黄芩苷在4.0×10-6~1.0×10-4mol.L-1浓度范围内与峰电流呈良好的线性关系,相关系数r=0.9991。方法检出限为8.2×10-7mol.L-1（S/N=3）。连续测定4.0×10-5mol.L-1的野黄芩苷溶液,RSD为1.8%（n=11）。该方法已成功地应用于注射液和片剂中野黄芩苷的测定。