HPLC法测定散结镇痛胶囊中三七皂苷R1、人参皂苷Rg1及人参皂苷Rb1的含量

目的：建立散结镇痛胶囊中三七皂苷R1和人参皂苷Rg1及人参皂苷Rb!的含量测定方法。方法：通过水饱和正丁醇提取和氢氧化钠溶液萃取制备供试品溶液,并采用HPLC法进行含量测定。结果：三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1质量的线性范围分别为0．3080—6．160μg（r=0．9999）、1．072—21．43μg（r=0．9999）和0．6245—12．49μg（r=0．9998）,平均回收率分别为96．03％、98．83％和97．13％,RSD分别为3．44％、1．58％和2．13％。结论：本法专属性、重现性好,可用于散结镇痛胶囊中三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1含量测定。     

三七总皂苷中各组分含量测定方法的改进

目的用薄层扫描法(TLSC)和高效液相色谱法(HPLC)测定三七总皂苷中人参皂苷Rb1(Rb1)、人参皂苷Rg1(Rg1)和三七皂苷R1(R1)3种主要成分的含量,并对两种方法进行比较,为修订质量标准中含量测定方法及含量限度提供依据。方法TLSC法用正丁醇-乙酸乙酯-水(4∶1∶5)上层溶液为展开剂,27%硫酸无水乙醇溶液为显色剂,测定波长λs=535 nm,λR=460nm;HPLC法用C18色谱柱,以乙腈-水线性梯度洗脱,0 min(25∶75)~15 min(45∶55);流速1.5 ml.min-1;测定波长200 nm。结果TLSC法测得三七总皂苷原料中Rb1、Rg1、R1的含量分别为31.07%、23.30%、9.35%;HPLC法测得三七总皂苷原料中Rb1、Rg1、R1含量分别为30.46%、22.65%、5.83%。结论HPLC法能将多种皂苷很好地分离并检测,简便快速,减少了误差。其准确度和测定结果的稳定性均优于TLSC法。     

田琥胶囊的制备与质量控制

目的建立田琥胶囊制备工艺及其质量标准。方法采用半浸膏喷雾制粒法制粒后填充成胶囊剂,用薄层色谱法对三七和丹参进行定性鉴别,用高效液相色谱(HPLC)法对人参皂苷Rg1、人参皂苷Rb1及三七皂苷R1的总量进行含量测定,并制定性状、检查等标准。结果制备工艺可行,制定的薄层色谱法可专属性检测三七和丹参,人参皂苷Rg1、人参皂苷Rb1及三七皂苷R1进样量分别在1.6～8.0,1.6～8.0及0.4～2.0μg范围内与峰面积线性关系良好。结论该制剂处方合理,制备工艺简单,质量控制方法准确、全面,可用于田琥胶囊的质量控制。     

三七固体分散体滴丸制备工艺及质量研究

目的：确定三七滴丸的处方和制备工艺,并对其质量进行初步考察。方法：采用正交验进行三七滴丸的处方设计和工艺优化。利用薄层色谱(TLC)进行定性鉴别。以人参皂苷Rg1、人参皂苷Rb1为标准,运用双波长薄层扫描法对人参皂苷Rg1和人参皂苷Rb1进行含量测定。结果：三七总皂苷——PEG6000——硬脂酸——吐温-80为15：31：1：3组成处方,滴丸甲醇提取液在λs=510nm,λr=700nm,经外标二点法扫描测定,得三七皂苷的含量。结论：所得滴丸在溶散时限、丸重差异上均符合药典标准。双薄层扫描法含量测定简便、准确。     

芪七连胶囊的质量标准研究

目的:建立芪七连胶囊的质量标准。方法:采用薄层色谱(TLC)法对制剂中黄芪、黄柏、黄连进行鉴定。采用高效液相色谱法测定制剂中人参皂苷Rg1、人参皂苷Rb1和三七皂苷R1的含量。色谱柱为Shim-pack VP-ODS C18,流动相为乙腈-水(梯度洗脱),流速为1.0 ml/min,检测波长为203 nm,柱温为20℃。结果:黄芪、黄柏、黄连TLC图斑点清晰,分离度好。人参皂苷Rg1、人参皂苷Rb1和三七皂苷R1检测进样量线性范围分别为0.9~9、0.94~9.4、0.3~3.0μg(r≥0.999 5);精密度、重复性、稳定性试验的RSD<3.0%;加样回收率分别为96.08%~99.75%(RSD=1.52)、97.03%~99.75%(RSD=1.10)、96.38%~98.55%(RSD=0.90),n均为6。结论:该方法操作简便、重复性好,可用于芪七连胶囊的质量控制。     

薄层扫描法测定仙灵双保心胶囊中人参皂苷Rg1及人参皂苷Rb1之和的含量

目的：建立仙灵双保心胶囊中人参皂苷Rg1及人参皂苷Rb1之和的含量测定方法。方法：双波长薄层扫描法，硅胶G薄层板，展开剂：氯仿－醋酸乙酯－甲醇－水（15：40：22：10）10℃以下放置的下层溶液，显色方法:10%顺序 酸乙醇溶液。结果：人参皂苷Rg1线性范围1－5μg，人参皂苷Rb1线性范围1．07－5．35μg；人参皂苷Rg1平均回收率为99．8％，RSD为2．6％；人参皂苷Rb1平均回收率为98．7％，RSD为2．5％。结论：方法准确、可靠，为控制仙灵双保心胶囊的质量提供了科学依据。     

疏血通脉胶囊定性定量方法研究

目的建立疏血通脉胶囊定性定量研究方法。方法采用TLC法对制剂中的薤白、瓜蒌皮、冰片进行鉴别,采用HPLC法,对制剂中的人参皂苷Rg1、人参皂苷Rb1和三七皂苷R1进行含量测定。结果 TLC法可检出薤白、瓜蒌皮、冰片。人参皂苷Rg1、人参皂苷Rb1和三七皂苷R1的线性范围分别为0.102¹.020、0.0951.020、0.095⁰.950和0.0350.950和0.035⁰.350 mg·mL-1(r=0.999 9),平均回收率分别为98.9%、99.6%和100.4%,RSD分别为2.0%、1.7%和1.7%(n=6)。结论该方法操作简单可靠,专属性强,可用于控制疏血通脉胶囊的质量。     

黄芪三七胶囊质量标准的研究

目的：建立黄芪三七胶囊的质量标准。方法采用TLC法对制剂中的黄芪进行定性鉴别;采用HPLC法测定制剂中的人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1的含量。结果黄芪薄层色谱斑点清晰且阴性对照无干扰;人参皂苷 Rg1、人参皂苷 Rb1、三七皂苷 R1分别在线性0.67~6.7μg、0.41~4.1μg和0.16~1.6μg 范围内线性关系良好（ r=0.9991、0.9999、0.9992）,平均回收率为99.35%,101.25%和99.82%, RSD分别为1.22%,0.99%和0.95%（n=6）。结论所建立的定性、定量方法简便易行,重复性好,为黄芪三七胶囊提供了质量控制方法。     

HPLC-ELSD法测定消栓通络胶囊中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1的含量

目的 采用高效液相色谱蒸发光散射检测器(HPLC-ELSD)法测定消栓通络胶囊中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1的含量.方法 以乙腈-水为流动相梯度洗脱(0～12 min,水80％-65％),Hypersil ODS柱(4.6 mm×250 mm,5 μm)为固定相,流速为1.0 mL·min-1,ELSD参数:漂移管温度:45℃,载气流量:1.5L·min1.结果 三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1的回收率分别为96.7、96.4％和97.7％,RSD分别为1.6％、1.4％和2.2％.结论 该方法简便、快速、重现性好,可用于消栓通络胶囊的质量控制.     

HPLC法测定活血舒脉胶囊中人参皂苷Rg_1、Rb_1及三七皂苷R_1的含量

目的考察活血舒脉胶囊中人参皂苷Rg1、Rb1及三七皂苷R1的含量,为制订活血舒脉胶囊质量标准提供科学的实验依据。方法采用HPLC法对10个批号的活血舒脉胶囊中人参皂苷Rg1、Rb1及三七皂苷R1进行含量测定。结果10批样品中人参皂苷Rg1、Rb1、三七皂苷R1最低含量分别为14.862、14.258、2.864mg.g-1;RSD分别为2.53%、1.12%、2.11%。结论10批样品测定结果表明各成分含量稳定,RSD均小于3.0%,可以作为制订活血舒脉胶囊质量标准的依据。     

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.

---

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。