UPLC-QqQ-MS/MS同时测定香槟方中4个生物碱成分

目的:建立超高效液相色谱-三重四极杆质谱法(UPLC-QqQ-MS/MS)同时测定香槟方中槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱的含量,比较槟榔、乌药单煎液与香槟方合煎液中4种生物碱成分的含量变化,为香槟方制剂研究提供实验基础。方法:采用Waters ACQUITY UPLC BEH Shield RP18色谱柱(2.1 mm×150 mm,1.7μm);流动相0.1%甲酸水溶液-乙腈梯度洗脱,流速0.2 mL·min-1,柱温30℃;采用电喷雾离子源(ESI),正离子模式扫描,多反应监测(MRM)模式检测;各化合物的定量离子对分别为m/z 142.10/44.11(槟榔次碱),156.20/44.07(槟榔碱),314.29/265.12(去甲异波尔定),328.13/265.10(波尔定碱)。结果:槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱分别在0.479 0～57.48,0.976 0～78.08,0.812 0～64.96,0.091 2～18.24μg·L-1线性关系良好(r≥0.994 8),平均加样回收率为93.73%～104.34%,RSD均5%(n=6)。香槟方中槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱的质量分数分别为(90.07±1.26),(445.27±12.39),(742.35±38.39),(38.50±3.33)μg·g-1,均显著低于单煎液中的含量。结论:该方法快速、灵敏、准确、重复性好,可用于香槟方中生物碱成分的含量测定,为香槟方的质量控制及深入研究提供参考依据;香槟方配伍对槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱的溶出量具有显著影响。     

Acetylcholinesterase inhibitory potential of a carbazole alkaloid,mahanimbine, from Murraya koenigii

In the search for acetylcholinesterase (AChE) inhibitors from Indian medicinal plants, via bioassay‐guided isolation, a carbazole alkaloid, mahanimbine [3, 5‐dimethyl‐3‐(4‐ methylpent‐3‐enyl)‐11H‐pyrano [5, 6‐a] carbazole], was isolated from the petroleum ether extract of the leaves of Murraya koenigii. Inhibition of AChE was evaluated based on Ellman's method using 96‐well microplate readers. Mahanimbine inhibited AChE activity in a dose‐dependent manner with an IC₅₀ value of 0.03 ± 0.09 mg/mL, while galantamine was used as a standard. The AChE inhibitory activity of this carbazole alkaloid has not been reported so far, and this study is the first to reveal this activity in carbazole alkaloid mahanimbine, isolated from Murraya koenigii. Copyright © 2009 John Wiley & Sons, Ltd.     

交泰丸有效部位自微乳系统的体内外评价

目的:对交泰丸有效部位自微乳化释药系统质量及大鼠在体肠吸收进行评价。方法:考察交泰丸有效部位自微乳液的外观、自微乳化后微乳粒径分布、外观、形态、类型、自乳化时间、药物含量及自微乳、微乳化后的稳定性;以黄连总碱为指标,运用大鼠在体肠回流模型,分析比较交泰丸有效部位制备自微乳前后对大鼠在体肠吸收的改善。结果:交泰丸有效部位自微乳化后微乳平均粒径为34.12 nm,可在3 min内基本乳化完全;自微乳液在室温下放置3个月较稳定;自微乳化后的微乳液在37℃下0.1 mol.L-1HCl溶液中放置8 h,交泰丸有效部位自微乳液与有效部位溶液剂比较,黄连总碱在体肠灌流液中的相对剩余百分含量(T)和表观吸收速率常数(Ka)值均获得明显提高(P0.01),前者的Ka是后者的152.6%。结论:自微乳化给药系统能显著改善交泰丸有效部位中黄连总碱大鼠小肠吸收,增加肉桂油在制剂中的稳定性。适合难溶性和难吸收药物的口服吸收,提高其生物利用度,是具有良好应用前景的中药制剂新剂型。     

海南萝芙木季胺碱——大斯配加春的结构

从海南萝芙木生产“降压灵”的母液中,分得一新的二聚体生物碱,命名为大斯配加春(macrospegatrine)。根据红外、紫外、质谱、氢谱及单晶X—射线衍射确定结构为Ⅰ式(图1)。     

Analysis of Vascular Endothelial Growth Factor (VEGF) and a receptor subtype (KDR/flk-1) in the liver of rats exposed to riddelliine: a potential role in the development of hemangiosarcoma

Riddelliine alters hepatocellular and endothelial cell kinetics and function including stimulating an increase in hepatocytic vascular endothelial growth factor (VEGF) in the absence of increased serological levels of VEGF (Nyska etal. 2002). The objective of this study was to further assess hepatic VEGF and KDR/flk-1 synthesis and expression by hepatic cells under riddelliine treatment conditions. Forty-two male F344/N rats were dosed by gavage with riddelliine (0, 1.0, and 2.5 mg/kg/day) for 6 weeks. Seven animals/group were sacrificed after 8 consecutive daily doses; remaining rats were terminated after 30 daily doses, excluding weekends. Hepatic tissues were evaluated by immunohistochemistry and in situ hybridization. The results showed that VEGF mRNA expression was observed in control and treated animals; however, qualitative differences were noted. Treated animals exhibited VEGF mRNA in clustered, focal hepatocytes and bile duct epithelium, whereas VEGF mRNA in hepatocytes from vehicle control rats was distributed evenly across all hepatocytes. Results evaluating the distribution of the VEGF cognate receptor, KDR/flk-1 showed that randomly distributed, rare sinusoidal endothelium, including those demonstrating karyomegaly and cytomegaly expressed KDR/flk-1. Phosphorylation of KDR/flk-1 at pTyr996 and pTyr1054/1059, but not pTyr951, was also detected, evidence that endothelial cell KDR/flk-1 was activated. These results suggest that both hepatocytes and endothelial cells are targets of riddelliine-induced injury. We speculate that damage to both populations of cells may lead to dysregulated VEGF synthesis by hepatocytes and activation of KDR/flk-1 by endothelium leading to the induction of sustained endothelial cell proliferation, culminating in the development of hepatic hemangiosarcoma.     

分光光度法测定抗风痛胶囊中总生物碱的含量

目的：采用分光光度法对抗风痛胶囊中总生物碱进行含量测定。方法：采用将生物碱变成盐酸生物碱，再和溴麝香草酚蓝络合反应后，用氯仿萃取出总生物碱比色测定。结果：与HPLC法测定结果相比，分光光度法对抗风痛胶囊中总生物碱进行含量测定结果可靠。结论：本方法能够作为抗风痛胶囊质量控制方法之一。     

浙贝母实生鳞茎中总生物碱含量的测定

测定了中药浙贝母不同生长年限、不同品种及不同栽培地点实生鳞茎中总生物碱的含量,结果表明符合药典要求,可供药用,为有性繁殖应用于生产提供依据。     

Fagaronine,a novel antileukaemic alkaloid

A review is presented about fagaronine, a benzophenanthridine alkaloid responsible for antitumoural activity. Plant source, extraction, biosynthesis, medicinal properties, especially antileukaemic activity, are described.     

川山橙中的一个新双吲哚生物碱,demethyltenuicausine

从川山橙(Melodinus hemsleyanus)中分离得到一个新双吲哚生物碱demethylteuicausine(I),通过光谱分析和半合成鉴定其结构,药理筛选表明其有一定的抗肿瘤活性。     

薄层扫描法对四逆汤配伍作用的化学分析

应用薄层扫描法对不同配伍“四逆汤”的3种乌头生物碱毒性成分进行测定,认为甘草对附子确有高度显著的佐制作用,干姜也有类似甘草的佐制作用,但效力次之。甘草、干姜交互作用亦高度显著。