藏药榜嘎中的双酯型和内酯型生物碱分析方法研究

目的建立藏药榜嘎中双酯型和内酯型生物碱的测定方法,为榜嘎的质量标准提高提供参考。方法采用高效液相色谱法。色谱柱为:Phenomenes luna C18(250mm×4.6mm,5μm);流速:1.0mL·min-1。双酯型生物碱的流动相为:A为乙腈-四氢呋喃(25∶15),B为0.1mol·L-1醋酸铵溶液(每1 000mL加冰乙酸0.5mL),梯度洗脱;检测波长为235nm;柱温为室温。内酯型生物碱的流动相为甲醇-水-氯仿-三乙胺(70∶30∶2∶0.1);检测波长230nm;柱温30℃。结果榜嘎中均不含新乌头碱、乌头碱、次乌头碱等双酯型生物碱;内酯型生物碱:阿替新在2.024²0.24μg范围内线性关系良好,线性方程:Y=1.918×104 X-678(r=0.999 9),平均回收率97.3%,RSD=0.9%;异叶乌头碱在2.00820.24μg范围内线性关系良好,线性方程:Y=1.918×104 X-678(r=0.999 9),平均回收率97.3%,RSD=0.9%;异叶乌头碱在2.008²0.08μg范围内线性关系良好,线性方程:Y=1.602×104 X-215(r=0.999 9),平均回收率98.6%,RSD=1.4%。结论该方法准确,可靠,专属性强,可用于榜嘎的质量控制。     

乳腺增生丸质量标准研究

目的对乳腺增生丸的质量标准进行研究。方法采用薄层色谱法同时鉴别乳腺增生丸中鸡血藤、当归、蒲公英3味药材。采用HPLC法三波长同时测定乳腺增生丸中绿原酸、咖啡酸、芍药内酯苷、芍药苷、阿魏酸和丹酚酸B的含量。色谱柱C18(4.6 mm×250 mm,5μm);以乙腈-水(含0.1%磷酸)为流动相梯度洗脱,流速1.0 mL/min;检测波长:绿原酸、咖啡酸、阿魏酸为320 nm,芍药苷、芍药内酯苷为230 nm,丹酚酸B为280 nm;柱温35℃;进样量20μL。结果薄层色谱斑点清晰,阴性对照无干扰。绿原酸、咖啡酸、芍药内酯苷、芍药苷、阿魏酸、丹酚酸B分别在10.0⁷0.0、2070.0、20¹40、55140、55³85、42385、42²94、10.0294、10.0⁷5.0、25075.0、250¹ 750μg/mL范围内呈良好的线性关系,平均回收率、RSD分别为100.5%、5.9%,100.2%、3.8%,101.2%、1.4%,99.9%、5.1%,100.6%、1.9%,99.8%、3.7%。结论方法准确可靠、重现性好,能有效控制乳腺增生丸的药品质量,为完善和提高乳腺增生丸质量标准提供了依据。     

淫羊藿中化学成分的UPLC/Q-TOF-MS分析

目的建立淫羊藿Epimedium brevicornu中化学成分的超高压液相色谱–飞行时间质谱(UPLC/Q-TOF-MS)的分析方法。方法 Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),流动相为0.1%甲酸水溶液–乙腈,梯度洗脱;体积流量为0.4 mL/min;柱温为45℃;进样量为2μL。质谱检测采用正、负离子模式,电压分别为3.0、2.5 kV;离子源温度110℃;雾化温度400℃;雾化气体积流量800 L/h。结果在10 min内完成淫羊藿中40个化学成分的鉴定。结论建立了一种简单、快速、高效的UPLC/Q-TOF-MS方法对淫羊藿中化学成分进行了鉴定,为全面控制淫羊藿的质量和机理研究提供了基础。     

荆芥挥发油的提取及包合工艺研究

目的:采用水蒸气蒸馏法提取荆芥挥发油,优选提取工艺及包合工艺。方法:以挥发油的提取量为考察指标,以加水量、浸泡时间、提取时间作为考察的3 个主要因素,通过 L9(34) 正交试验法优化荆芥挥发油最佳提取工艺。以挥发油与β-环糊精的比例、溶剂用量、时间为考察因素,优选挥发油的包合工艺。结果:最佳提取工艺为饮片加水12倍量,浸泡3小时,提取8小时; 最优包合工艺为挥发油与β-环糊精比例为1:10,加入溶剂量为3倍量,胶体磨碾磨时间为15min。结论:优选的提取工艺和包合工艺简便、快速、稳定、可行,可作为荆芥挥发油产业化生产工艺。     

A new labdane-type diterpenoid from Leonurus japonicus

Five fractions prepared from the crude extract of Leonurus japonicus were examined in order to determine their cytotoxic potential. Under the bioassay guidance, a new labdane-type diterpenoid (1), and nine known ones (2–10) along with a seco-labdane (11) were isolated from the aerial parts of Leonurus japonicus. The structure elucidation was primarily based on comprehensive spectroscopic analyses, including HRESIMS, IR, and 1D and 2D NMR methods. Compound 4 (6β-hydroxy-15,16-epoxylabda-8,13(16),14-trien-7-one) exhibited potential cytotoxicity against HeLa cell line (IC₅₀ = 23.75 μM).     

米索前列醇联合益母草注射液与单纯使用益母草预防产后出血疗效比较

目的寻找一种更有效、简便、实用的方法预防和治疗产后出血。方法将足月妊娠阴道分娩、非高危妊娠、无前列腺禁忌证产妇120例随机分2组,观察米索前列醇联合益母草注射液与单纯使用益母草注射液对产后2h内阴道出血的疗效比较,实验组60例,于胎头娩出后立即舌下含服米索前列醇200ug并肌注益母草注射液1mL;对照组60例,于胎头娩出后肌注益母草注射液1mL。结果实验组第三产程时间较对照组缩短(P<0.01),产后2h内平均出血量较对照组减少(P<0.01)。结论应用米索前列醇联合益母草注射液比单纯使用益母草注射液能更好地促进子宫收缩,减少产后出血,是一种安全、有效防治产后出血的方法。     

Hepatoprotective effects of Artemisiae Capillaris Herba and Picrorrhiza Rhizoma combinations on carbon tetrachloride–induced subacute liver damage in rats

The hepatoprotective properties of Artemisiae Capillaris Herba (AC) and Picrorrhiza Rhizoma (PR) are well known. The aim of this study was to determine the optimal composition of AC and PR mixtures for better complimentary or alternative regimens in reducing the level of hepatic fibrosis. Ten weeks of carbon tetrachloride injections caused subacute hepatic damage, manifested as significantly less body weight gain and hepatic protein content, and a higher liver weight, serum aspartate aminotransferase and alanine aminotransferase levels, hepatic malondialdehyde (an index for lipid peroxidation), and hydroxyproline (an index for collagen synthesis) concentrations. The carbon tetrachloride–induced toxic effects were inhibited by 11 different AC/PR mixtures as well as the single AC or PR treatment. More favorable effects were detected in all mixed-formulation groups compared with the AC or PR single formulations. Moreover, the AC/PR 2:1 formulation showed the most favorable hepatoprotective activity. The AC and PR mixtures showed good synergic hepatoprotective activity that was attributed to increasing free-radical scavenging ability. Among the 11 types of mixed formula tested in this study, the AC/PR 2:1 formulation had the most impressive synergic effects on inhibiting the subacute hepatic damage induced by carbon tetrachloride in rats and showed more favorable effects than with an equal dose of silymarin.     

鲜鱼腥草提取物对脂多糖所致小鼠肺部炎症的影响

目的研究鲜鱼腥草提取物对脂多糖所致小鼠肺部炎症的影响。方法采用ICR小鼠鼻滴脂多糖(LPS)建立肺部炎症模型,检测小鼠支气管肺泡灌洗液(BALF)中炎症细胞数和病理学观察肺组织炎症程度。结果鲜鱼腥草提取物40～400mg·kg-1可减少小鼠LPS所致的BALF中白细胞增高,还可减轻肺组织病理炎症细胞浸润。结论鲜鱼腥草提取物可以减轻LPS所致的小鼠肺部炎症反应,减少炎症细胞浸润。提示鲜鱼腥草提取物对脂多糖所致小鼠肺部炎症有抑制作用。     

攀枝花地区鱼腥草挥发性化学成分的气相色谱-质谱联用分析

目的对产自攀枝花地区鱼腥草中挥发油进行提取,同时分析鉴定其化学组分,确定各成分的相对含量。方法采用普通水蒸气蒸馏萃取法提取挥发油,用气相色谱-质谱联用技术分析鉴定挥发油化学组分,应用峰面积归一化法确定各成分的相对含量。结果测得鱼腥草挥发油含量为0.97%,鉴定出13种化学组分,占挥发性物质总含量的91.40%。结论普通水蒸气蒸馏萃取法提取的挥发油中主要含有邻苯二甲酸二辛酯(23.49%)、4-甲基-1-(1-甲基乙基)-3-环己烯-1-醇(16.81%)、(E)-9-十八碳(烯)酸(10.00%)、β-蒎烯(8.64%)。     

高效液相色谱法测定一点红中槲皮素的含量

目的建立高效液相色谱法测定一点红中槲皮素含量的方法。方法用Hypersil BDS C18色谱柱(4.6 mm×200 mm,5μm),流动相为甲醇-水-磷酸(55∶45∶0.4),检测波长为370 nm。结果槲皮素在0.041 6~0.416μg的范围内与峰面积呈良好线性关系(r=0.999 8),平均加样回收率为102.3%,RSD为1.18%(n=6)。结论此法用于测定一点红中槲皮素的含量快速、简便、准确,为评价一点红的内在质量提供了科学依据。