益母黄丹口服液的制备工艺研究

确定益母黄丹口服液的制备工艺条件并建立质量标准。采用正交试验法,对益母黄丹口服液的提取制备工艺条件进行优化,并采用紫外分光光度法,以盐酸益母草碱为对照品,在277 nm处测定按照不同工艺制备的口服液中盐酸益母草碱含量,再采用薄层色谱法对口服中益母草、黄精进行定性鉴别进行质量控制。结果表明,口服液最佳制备工艺为煎煮时间1.5 h,煎煮3次,醇沉分数50%;紫外分光光度法能测定口服液中益母草碱含量、薄层色谱中益母草、黄精斑点清晰,阴性对照无干扰。本试验制备工艺的方法简单可行,建立的质量标准适用于益母黄丹口服液的质量控制。     

山药对免疫机能低下小鼠耐缺氧能力的影响

探讨山药对氢化可的松(HC)诱导的免疫机能低下小鼠耐缺氧能力的影响。按析因分析法设计2×2因子,将40只小鼠分为对照组(A),模型组(B),用药组(C),低下用药组(D),B、D组每天腹腔注射HC(20mg/kg),连续21d;自第4天开始,D组注射HC的同时,C、D组每天灌胃山药水煎液(50mg/kg);A、B组灌胃等量蒸馏水;第22天进行常压密闭耐缺氧试验,记录小鼠存活时间,后处死小鼠迅速称其脾脏、胸腺重量,计算脾指数、胸腺指数,常规石蜡切片,HE染色。结果显示,山药可延长免疫机能低下小鼠的缺氧耐受时间,提高脾指数、胸腺指数(P0.05),改善胸腺脾脏的组织结构。山药对HC有一定的颉颃作用。     

菌痢消颗粒薄层色谱研究

菌痢消颗粒是由黄连、诃子、苦参、白头翁、甘草等中药制成的纯中药制剂,具有清热燥湿,泻火解毒,涩肠止泻之功效。在对本品的质量标准研究中,本文重点进行了薄层色谱研究,选择了多种展开系统进行比较。结果显示,采用《中国兽药典》收载方法及展开系统对本方中黄连、诃子、苦参进行薄层色谱鉴别,斑点清晰,方法可行。     

禹白附抗肿瘤活性成分研究(Ⅱ)

应用溶剂提取法、萃取法和柱色谱技术对禹白附的化学成分进行提取分离。根据波谱数据(1HNMR、13CNMR、MS、IR)和理化性质鉴定了2个化合物的结构,分别为对乙酰氨基酚(1)、β-谷甾醇(2)。化合物1为首次从该植物中获得,本研究为进一步开发利用禹白附提供了科学依据。     

Cytotoxicity and antihyperglycemic effect of minor constituents from Rhizoma Coptis in HepG2 cells

Generally, berberine, coptisine, palmatine, and jatrorrhizine were considered as the main bio-active compounds in Rhizoma Coptis (RC). Little attention was paid to investigate the pharmacological activity of minor constituents in RC. The present study was designed to separate the minor compounds, and the cytotoxicity and antihyperglycemic effect of these compounds in HepG2 cells were also studied. Palmatine (1), berberine (2), coptisine (3), epiberberine (4), columbamine (5), and jatrorrhizine (6) from RC ethanol extract were isolated by high speed counter current chromatography (HSCCC) in one run. The remaining fraction (about 50% of extract in HSCCC) was further isolated by traditional column chromatography methods to yield magnoflorine (7), ferulic acid (8), and choline (9). Another four alkaloids, namely groenlandicine (10), berberrubine (11), oxyberberine (12), 8-oxo-coptisine (13), also were obtained from CHCl₃ extracts. Especially, choline was first isolated from RC. Cell assay indicated that the minor fractions excluding compounds 1-6 showed obvious glucose lowering activity. In addition, the minor monomers also exhibited moderate glucose lowering activity. The combination of berberine and ferulic acid showed synergistic effect on antihyperglycemic. The combination of alkaloids 1-6 was same so. All compounds had different cytotoxicity in HepG2 cells within the test concentration. Of them, berberrubine showed the strongest cytotoxicity. The results suggested that combined action of variety constituents contributed to the antihyperglycemic effets and low cytotoxicity of RC extract in HepG2 cells.     

Occurrence of stilbene oligomers in Cyperus rhizomes

Investigation of the chemical constituents of Rhizoma Cyperi (Cyperus rotundus Linneus) resulted in the isolation of novel enantiomeric and meso-stilbene trimers [i.e., (+)- and (−)-(E)-cyperusphenol A (1, 2 respectively) and (E)-mesocyperusphenol A (3)], a trimer bearing a novel hexacyclic ring system [cyperusphenol B (5)], as well as known stilbenoids (cyperusphenols C (4) and D (6), scirpusins A (7) and B (8), and piceid (9)) and luteolin. HPLC was used for the optical resolution of 1 and 2 as well as for the identification of cooccurrence of enantiomers of 7. The structures of the isolates were established by spectroscopic analyses, including a detailed NMR spectroscopic investigation. The isolates were evaluated in terms of their antiproliferative activity employing the Jurkat cell line (human T-cell leukemia cells), while the IC₅₀ potencies of a racemate of 1 and 2, 3, 5, and 6 were estimated as 27.4, 40.5, 26.4, and 26.3 μM, respectively. The suppression of cell growth by 6 was due to the induction of apoptosis, which was characterized by nuclear changes and PARP-1 cleavage determined by western blotting. We also evaluated the free radical scavenging activity of the isolates.     

白芍和黄连中十五种有机氯和拟除虫菊酯类 农药的多残留分析方法

建立了白芍和黄连两种中药材中六六六、滴滴涕、艾氏剂、五氯硝基苯、甲氰菊酯、氯菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯等农药的多残留气相色谱分析方法。在索氏提取器中以石油醚(60~90℃)为溶剂提取样品,提取液经氧化铝与弗罗里硅土的混合柱净化,采用农残分析专用柱农残Ⅱ 柱分离,GC-ECD检测器检测农药的残留量。方法的最小检出量(LOD)为0.000 5~0.006 0 ng, 最低检测浓度(LOQ)为0.005~0.050 mg/kg;3个添加水平农药的平均回收率为79.8％~114.6％,相对标准偏差(RSD)均小于10％ (n=6) 。     

黄连盐酸小檗碱对照品的制备

采用硅胶柱层析和重结晶等方法对黄连50％乙醇提取物进行分离纯化.通过熔点测定、HPLC、质谱等对自制的盐酸小檗碱对照品进行结构确证,采用TLC和HPLC进行对照品纯度检测.所制备的盐酸小檗碱对照品经TLC检查无杂质斑点,采用HPLC面积归一化法测定其含量达98.97％.表明该方法制备的盐酸小檗碱对照品纯度高,符合中药化学对照品的相关技术要求,可作为黄连药材及其制剂质量控制用的化学对照品.     

不同种源延胡索及土壤中有机氯农药残留特征及安全评价

以万州、开县实验基地土壤和9个种源延胡索为研究对象,使用气相色谱–电子捕获检测器(GC-ECD)检测了土壤和延胡索中有机氯农药(OCPs)残留量,分析其残留特征和生态安全。结果表明:①在土壤和延胡索样品中均检出了滴滴涕(DDTs)和六六六(HCHs),DDTs的检出率分别为100%和83.3%,HCHs的检出率分别为72.2%和100%。DDTs和HCHs残留量具有较大的离散性和一定的区域差异性。②在土壤样品中,检出率较高的是4,4'-DDE和α-HCH,分别为100%和66.7%。4,4'-DDE和α-HCH是OCPs残留的主要成分。③在延胡索样品中,检出率较高的是α-HCH、4,4'-DDE和β-HCH,分别为100%、77.8%和55.6%,3种成分占OCPs残留量的73.7%。延胡索对α-HCH和4,4'-DDE有很强的生物富集作用,富集因子分别约为1.8和0.65。④实验基地土壤OCPs残留符合《土壤环境质量标准》二级标准,属于尚清洁水平,延胡索的OCPs残留量符合《药用植物及制剂外经贸委绿色行业标准》。