自拟四味止血片质量标准的改进和完善

目的建立四味止血片的质量标准。方法采用薄层色谱法(TLC法)对四味止血片中益母草、地榆、丹参进行定性鉴别;采用高效液相层析(HPLC)测定丹参中丹参素钠的含量,色谱柱:Agilent SB-C_(18)(4.6×250 mm,5μm),流动相:乙腈-2%冰乙酸溶液(5∶95),流速0.8 ml/min,检测波长281 nm,柱温25℃。结果薄层鉴别中,供试品在与对照药材或对照品相应的位置上显相同颜色的斑点,阴性对照无干扰;丹参素钠的线性范围0.3980~3.9800μg,r=0.9999(n=7),平均回收率95.31%,RSD为2.17%(n=9)。结论该方法操作简便,结果准确可靠,重复性好,可作为四味止血片的质量控制方法。     

活血止痛片质量控制方法研究

目的 研究活血止痛片质量控制方法.方法 采用TLC对活血止痛片中当归、三七、乳香、冰片和土鳖虫进行定性鉴别;采用HPLC对活血止痛片中的阿魏酸进行含量测定,色谱柱为 Hypersil ODS2(4.6 mm×250 mm,5 μm),流动相为甲醇-1%乙酸水溶液(30∶70),检测波长为320 nm,流速为1.0 mL·min-1.结果 薄层色谱鉴别专属性强,阿魏酸进样量在0.01～0.14 μg范围内线性关系良好(r=0.999 9),平均加样回收率为98.60%(RSD=0.64%).结论 本方法操作简便,结果可靠,重现性好,可用于活血止痛片的质量控制.     

冠心通胶囊质量控制

目的:建立冠心通胶囊质量控制方法。方法:采用TLC对冠心通胶囊中的川芎和三七药材进行定性鉴别;采用HPLC对冠心通胶囊中的丹参素进行含量测定,色谱条件:HypersilC18色谱柱(250mm×4.6mm,5μm),以甲醇-水-冰醋酸(8∶91∶1)为流动相,柱温:30℃,流速:1.0mL.min-1,检测波长:281nm。结果:川芎和三七药材的薄层色谱鉴别专属性强,丹参素进样量在0.052～0.52μg范围内与峰面积呈良好的线性关系(r=0.9998,n=6)。丹参素的平均回收率为100.83%,RSD为1.4%。结论:本方法可准确的进行定性、定量,可用于控制冠心通胶囊的质量。     

小儿泻痢片定性定量研究

目的建立小儿泻痢片定性定量研究方法。方法采用TLC法对葛根、黄连进行定性鉴别;采用HPLC法测定小儿泻痢片中黄芩苷的含量,选用Diamonsil C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水-磷酸(47∶53∶0.2),流速:1.0 mL·min-1,柱温30℃,检测波长280 nm。结果 TLC检出了葛根、黄连特征斑点,阴性无干扰;黄芩苷在0.075~0.60μg与峰面积线性关系良好(r=0.999 6);加样回收率为98.0%,RSD=1.9%。结论方法简便、稳定,可作为本品的定性定量方法。     

冠脉通片质量控制研究

目的建立冠脉通片的质量控制方法。方法采用TLC法,分别以甲苯-醋酸乙酯-甲酸(15∶2∶1)、乙酸丁酯-甲酸-水(1.3∶1∶1)10℃下放置的上层溶液为展开剂对何首乌及淫羊藿进行薄层色谱鉴别;采用气相色谱法,以水杨酸甲酯为内标物,安捷伦DB-WAX毛细管柱(30m×0.53mm,1μm),FID检测器,载气为氮气,柱温为140℃,测定冠脉通片中的冰片;采用高效液相色谱法,Dikma-C18色谱柱(250mm×4.6mm,5μm),甲醇-0.5%乙酸(88∶12)为流动相,体积流量1.0mL/min,检测波长281nm,柱温25℃,测定冠脉通片中的丹参素。结果薄层鉴别中样品色谱斑点清晰,分离较好;气相色谱中,冰片中龙脑及内标物水杨酸甲酯均得到良好的分离,冰片的平均回收率为96.72%(RSD为0.67%);HPLC测定丹参素在0.1008～0.6048μg与峰面积值线性关系良好(r=0.9998),平均回收率为100.22%(RSD为1.15%)。结论本实验建立的方法简便、准确、可靠,可用于冠脉通片的质量控制。     

心脉通片质量标准的研究

摘要：目的:建立心脉通片的定性鉴别方法和含量测定方法,以完善其质量标准。方法:采用TLC法对心脉通片中毛冬青、钩藤、夏枯草分别进行定性鉴别。采用HPLC法分别测定心脉通片中丹参素、橙黄决明素的含量:色谱柱分别为SymmetryShieldTMRP18、Thermo ODS Hypersil,流动相分别为甲醇-乙腈（30∶10）-0.5%甲酸溶液（梯度洗脱）、乙腈-0.1%磷酸溶液（25∶75）,检测波长分别为280 nm、284 nm,流速均为1.0 ml·min-1,柱温均为30℃,进样量分别为10μl、20μl。结果:TLC图谱斑点清晰,分离度好,阴性对照无干扰。丹参素钠、橙黄决明素的进样浓度线性范围分别为0.021～0.527 mg·ml-1（r=1.000 0）、0.236～18.894μg·ml-1（r=0.999 8）,平均回收率分别为98.5%（RSD=1.7%,n=6）,108.8%（RSD=0.5%,n=6）,精密度、稳定性、重复性试验的RSD均小于4.5%（n=6）。结论:研究建立的定性、定量方法准确可靠,能为心脉通片质量标准的提高奠定研究基础。     

薄芝片的质量控制标准研究

目的:建立薄芝片的质量控制方法。方法:采用 TLC 方法,使用4%磷酸氢二钠的羧甲基纤维素钠溶液为粘合剂的硅胶 GF_(254)(10～40 μm)薄层板,以甲苯-乙酸乙酯-甲醇-异丙醇-浓氨试液(12∶6∶3∶3∶1)为展开剂,对薄芝片中核苷类成分腺苷进行定性鉴别;采用 HPLC 法,使用 Alltima C_(18)色谱柱(250 mm×4.6 mm,5 μm),以乙腈-水(5∶95)为流动相,流速1.0mL·min~(-1),检测波长262 nm,柱温25 ℃,进样量20 μL,对薄芝片中的腺苷和尿苷同时进行含量测定。结果:腺苷的 TLC 鉴别专属性强;HPLC 测定,腺苷、尿苷的线性范围分别为0.12～0.62μg(r=0.9994,n=5)和0.18～0.88μg(r=0.9998,n=5),平均回收率(n=6)分别为99.22%(RSD=2.2%)和100.5%(RSD=2.0%)。结论:本方法简单、可靠、准确,可用于控制薄芝片的质量。     

复方丹参滴丸中丹参素的含量测定

目的建立高效液相法(HPLC)测定复方丹参滴丸中丹参素含量的方法。方法色谱柱为Nucleosil C18色谱柱(250×4.6mm,10μm),以甲醇-水-冰醋酸(21∶78∶1.0)为流动相;柱温为室温;流速为0.9 mL/min;检测波长为280 nm。结果丹参素对照品在0.01～0.10mg/mL范围内呈良好线性关系(r=0.997,n=5),回归方程为A=17371C+3500,平均回收率为100.15%,RSD为4.19%,所测复方丹参滴丸中丹参素的平均含量为8.034mg/g,符合2010版药典对其含量的要求。结论 HPLC测定复方丹参滴丸中丹参素含量的方法操作流程简单、快速,准确度高,建议在复方丹参滴丸的质量监控中大力推广使用。     

头痛安片质量标准研究

目的研究头痛安片质量控制方法。方法采用薄层色谱法对方中丹参、当归、白芍进行定性研究。采用HPLC法,以乙腈-1冰醋酸(9:91)为流动相,检测波长为280nm,应用EclipseXDBC18(4.6mm×250mm,5μm)柱,测定方中丹参的丹参素含量。结果丹参、当归、白芍可用薄层色谱鉴别,丹参素钠在0.2～3.2μg/mL范围内线性关系良好(r=0.9997),平均回收率为97.09,RSD为1.21(n=6)。结论本研究建立的质量标准方法简便、快捷,重现性好,可用于头痛安片的质量控制。     

HPLC法测定复方丹参滴丸中丹参素的含量

目的建立高效液相色谱法(HPLC)快速测定复方丹参滴丸中丹参素的含量。方法色谱柱为Hypersil C18(4.6 mm×250 mm,5μm);流动相为甲醇-水-冰醋酸(20∶80∶0.5),柱温为室温;流速为0.9 m L/min;检测波长为281 nm。结果丹参素对照品在0.01~0.10 mg/m L范围内呈良好线性关系,r=0.9997,含量丹参素平均回收率为99.6%,RSD为0.89%。所测复方丹参滴丸中丹参素的平均含量为8.034 mg/g,符合2010年版药典对其含量的要求。结论 HPLC法测定复方丹参滴丸中丹参素的含量方法操作流程简单、快速、准确,可用于该制剂的质量控制中大力推广使用。     

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.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

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.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.