HPLC法测定荷叶与莲房中荷叶碱的含量

目的建立高效液相色谱法测定荷叶与莲房中荷叶碱含量的方法。方法采用Agilent Eclipse XDBC18(4.6 mm×250 mm,5μm),以乙腈-水-三乙胺-冰醋酸(27∶70.6∶1.6∶0.8)为流动相;流速:1.0 mL·min-1;柱温:25℃;检测波长:270 nm。结果荷叶碱在3.01⁴8.16μg·mL-1范围内线性良好(r=0.999 0),平均回收率为96.97%,RSD=0.99%(n=6)。结论该方法准确、简便、灵敏度高、重现性好,可用于荷叶与莲房中荷叶碱含量的测定。     

高效液相色谱法测定荷叶中荷叶碱的含量

目的:建立 HPLC 测定荷叶中荷叶碱含量的方法。方法:采用 Symmetry-C_(18)柱(3.9mm×150mm,5μm),流动相为乙腈-水-三乙胺-冰醋酸(56∶44∶1∶0.15);流速:0.5mL·min~(-1);检测波长:270nm;柱温:25℃。结果:荷叶碱在3.00～15.00μg·mL~(-1)范围内具有良好的线性关系,r=0.9999,平均回收率为98.3%,RSD=2.1%(n=5)。结论:本法简便、准确,灵敏度高,重复性好,可用于荷叶成分的含量测定。     

HPLC法测定果蔬纤维颗粒中荷叶碱含量

目的:建立果蔬纤维颗粒中有效成分荷叶碱含量的高效液相色谱测定方法。方法:选用Hypersil C18柱(250mm×4.6 mm,10μm),以乙腈-水-三乙胺-冰醋酸(34∶63.6∶1.6∶0.78)为流动相,检测波长为270 nm,进样量为20μl,柱温为30℃。结果:荷叶碱进样浓度在0.588～5.88μg/ml范围内与峰面积线性关系良好,平均回收率为98.56%,RSD为1.13%(n=9),精密度高,重复性好。结论:所建立的果蔬纤维颗粒荷叶碱含量高效液相色谱测定方法,操作简便,结果准确,重现性好,可用于果蔬纤维颗粒中有效成分荷叶碱的含量测定。     

基于HPLC-QAMS同时测定荷叶水提物中6个成分的含量

目的:建立一测多评法(QAMS)同时测定荷叶水提取物中O-去甲荷叶碱、槲皮素-3-O-桑布双糖苷、金丝桃苷、异槲皮苷、槲皮素-3-O-葡萄糖醛酸苷、荷叶碱的含量。方法:色谱柱为Lamdo Stamsil C₁₈(250 mm×4.6mm, 5μm),流动相为0.1%磷酸水溶液-乙腈,梯度洗脱,流速为0.6 mL·min^-1,检测波长为270 nm,柱温为25℃,进样量为5μL。以O-去甲荷叶碱为内参物,计算其他5个成分的相对校正因子,并测定含量。结果:O-去甲荷叶碱、槲皮素-3-O-桑布双糖苷、金丝桃苷、异槲皮苷、槲皮素-3-O-葡萄糖醛酸苷、荷叶碱分别在各自范围内线性关系良好(r≥0.999 5),精密度、重复性、稳定性试验结果的RSD均<3.0%,平均加样回收率为94.6%～108.0%,RSD为0.95%～2.1%。QAMS法测得荷叶水提物中上述6个成分的含量分别为0.23、3.43、1.69、10.59、41.23、0.69 mg·g^-1。结论:建立的荷叶水提物中6个成分的含量测定方法可靠,可用于其质量控制...     

薄层扫描法测定荷叶中荷叶碱的含量

目的: 建立薄层扫描法分离测定荷叶中荷叶碱的含量.方法: 采用0.5%氢氧化钠溶液制备的硅胶GF254薄层板,以氯仿-醋酸乙酯-甲醇-水(30∶40∶20∶10)为展开剂,检测波长272 nm.结果: 荷叶碱在0.5～5 μg范围内呈现良好线性关系,平均回收率为97.4%,RSD=3.83%(n=5).结论: 该方法简便准确,稳定性高,可作为其质量控制依据.     

反相高效液相色谱法测定荷叶口服液中荷叶碱的含量

［摘要］目的建立高效液相色谱法测定荷叶口服液中荷叶碱含量。方法固定相：HypersilBDS C18柱 （4.6 mm×150 mm, 5 μm）;流动相：甲醇：水：三乙胺：冰醋酸（50：48：1.4：0.7）;流速：0.7mL&#8226;min 1;检测波长：270 nm;柱温：40 ℃;进样量：10 μL。结果荷叶碱在1.282～25.640 μg&#8226;mL 1范围内线性关系良好（r＝0.999 1）;3份荷叶碱的平均加样回收率分别为99.7%（RSD=1.25%）,101.0%（RSD＝0.95%）,99.5%（RSD＝1.14%）。结论该方法准确可靠,快速灵敏,可以作为荷叶口服液中荷叶碱的质量控制标准。     

反相高效液相色谱法测定通脉降脂片荷叶碱含量

目的建立测定通脉降脂片中荷叶碱含量的反相高效液相色谱法。方法色谱柱为Diamonsil ODS C18（250 mm×4.6 mm,5 μm）;流动相：乙腈 0.05%三乙胺（35：65）;流速：1.0 mL&#8226;min－1;检测波长270 nm;柱温：25 ℃;进样量：10 μL。结果荷叶碱在0.125～3.120 μg范围内线性关系良好（r=0.999 9）;平均回收率为99.66%,RSD为1.12%（n=6）。结论该检测方法可靠、准确、重现性好,可用于通脉降脂片中荷叶碱的含量测定。     

荷叶HPLC-UV指纹图谱研究

目的采用HPLC法建立荷叶药材的指纹图谱。方法 Ultimate XB-C18色谱柱(4.6 mm×250 mm,5μm),流动相为0.1%甲酸+0.2%三乙胺溶液(A)-乙腈(B)进行梯度洗脱,检测波长254 nm,体积流量1.0 mL.min-1,柱温35℃。结果建立了荷叶的HPLC-UV的指纹图谱,指定出11个共有指纹峰,共指认3个共有峰的结构并对不同产地和不同采收时期荷叶的相似度进行了比较。结论本方法操作简便,快速,重现性好,为荷叶的鉴别和质量控制提供有效依据。     

HPLC法同时测定泌感颗粒中小檗碱和槲皮素的含量

目的:建立同时测定泌感颗粒中小檗碱和槲皮素含量的方法。方法:采用高效液相色谱法,色谱柱为 Diamonsil C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液(27:73),流速为1.0 mL·min~(-1),检测波长为360nm。结果:小檗碱浓度在8.33～41.6μg·mL~(-1)范围内线性关系良好(r=0.9997),平均方法回收率(n=6)为98.6%;槲皮素浓度在4.08～20.4μg·mL~(-1)范围内线性关系良好(r=0.9998),平均方法回收率(n=6)为97.8%;结论:本法简便,准确度和重复性好,可用于泌感颗粒中小檗碱和槲皮素的同时测定。     

RP-HPLC同时测定四季三黄软胶囊中黄芩苷和盐酸小檗碱的含量

目的建立RP-HPLC法同时测定四季三黄软胶囊中黄芩苷和盐酸小檗碱的含量.方法采用色谱柱为hypersil BDSC18(250 mm×4.6 mm,5μm),以乙睛-0.5%三乙胺水溶液(磷酸调pH至3.1)(2575)为流动相,检测波长265 nm,流速1.0ml·min-1.结果黄芩苷在1.6-206 lag·ml-1范围内,线性关系良好(r=0.999 9),平均回收率为100.3%.RSD=1.7%(n=6);盐酸小檗碱在1.6-208μg·m1-1范围内,线性关系良好(r=0.999 9),平均回收率为100.8%,RSD=1.6%(n=6).结论该方法结果准确可靠,重现性好,可用于四季三黄软胶囊的质量控制.     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

Glycofection: The Ubiquitous Roles of Sugar Bound on Glycoplexes

Glycofection (transfection by using sugar-substituted polylysine) was assessed in order to provide an alternative to viral vectors for the transfer of genes into vascular smooth muscle cells. A rabbit vascular smooth muscle cell line (Rb-1 cells) was selectively transfected by using glycoplexes (glycosylated polylysine/pSV2LUC complexes) in the presence of 10 mu M of the fusogenic peptide GALA. A sugar-specific transfection was obtained when the glycofection was conducted for 1 h with glycoplexes containing either alpha Gal, alpha -Glc, alpha -GalNAc, beta -GlcNAc, or beta -GalNAc residues. The gene expression was high after transfection, with glycoplexes bearing alpha Gal, alpha -GalNAc, or beta -GalNAc residues that were weakly internalized, and low with glycoplexes carrying Lact or Rha residues that were well taken up by cells. These results suggest that 1) glycofection can be a good approach for a selective transfer of genes intovascular smooth muscle cells, 2) an efficient uptake of the glycoplexes is not the unique limiting step for an efficient transfection, and 3) the sugar-dependent trafficking of the glycoplexes inside the cells may account for the transfection efficiency.     

直肠癌下切缘病理组织学分析

目的探讨直肠癌逆向浸润与下切缘的安全距离的关系。方法对36例直肠癌Miles手术和Dixon手术后标本的肿瘤下缘1.0cm、2.0cm、3.0cm的肠壁及对应的系膜病理组织学检查,观察直肠癌逆向浸润或转移的距离。结果36例直肠癌标本距癌肿下缘1.0 cm、2.0cm、3.0cm的肠壁及对应的系膜病理组织学检查均为阴性,结论直肠癌远恻逆向浸润或转移未见超过1.0cm,因此认为保肛手术时切除肿瘤远侧肠管(包括系膜)2.0cm是安全的。