一测多评法测定丹酚酸A原料药中迷迭香酸、紫草酸、丹酚酸B和丹酚酸C

目的建立一测多评法测定丹酚酸A原料药中特定杂质迷迭香酸、紫草酸、丹酚酸B和丹酚酸C。方法采用Agilent Zorbax Eclipse XDB-C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相0.2%磷酸–乙腈,梯度洗脱,检测波长286 nm,体积流量1.0 mL/min,柱温25℃,样品室温度4℃,进样量20μL。以丹酚酸A为内标,建立丹酚酸A原料药中特定杂质(紫草酸、迷迭香酸、丹酚酸B、丹酚酸C)的相对校正因子;分别采用一测多评法和外标法测定丹酚酸A原料药中特定杂质,并比较一测多评法计算值与外标法实测值的差异性。结果丹酚酸A、丹酚酸B、丹酚酸C、迷迭香酸、紫草酸均在0.2~20μg/mL与峰面积呈良好线性关系。在线性浓度范围内,迷迭香酸、紫草酸、丹酚酸B、丹酚酸C与丹酚酸A间的相对校正因子分别为1.52、2.09、2.33、1.06。一测多评法计算值与外标法实测值无显著性差异。结论一测多评法可用于丹酚酸A原料中迷迭香酸、紫草酸、丹酚酸B、丹酚酸C的测定。     

HPLC法测定生骨胶囊中丹酚酸B的含量

目的:建立用高效液相色谱法测定生骨胶囊中丹酚酸B含量的方法.方法:采用Agilent-C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-甲酸-水(35∶1∶64),柱温为28℃,流速为1.0 ml·min-1,检测波长为286 nm.结果:丹酚酸B进样量在0.096 ～1.435μg范围内与峰面积线性关系良好,平均回收率为101.6％,RSD为0.7％(n=9).结论:所用方法简便、快捷、准确,可作为生骨胶囊中丹酚酸B的含量测定方法.     

反相高效液相色谱梯度洗脱法测定安神补心片中丹参酮ⅡA和丹酚酸B含量

目的 测定安神补心片中丹参酮ⅡA和丹酚酸B的含量.方法 采用Diamonsil C18柱(250 mm×4.6 mm,5 μm),梯度洗脱,流动相A为乙腈、B为水、C为甲醇、柱温35℃,检测波长为270 nm.结果 丹参酮ⅡA进样量在0.013 21～0.264 2μg范围内,丹酚酸B进样量在0.061 10～1.222 0μg范围内与峰面积均有较好的线性关系,加样回收率丹参酮ⅡA为98.60%,丹酚酸B为98.58%.结论 该方法结果准确、快速,可作为安神补心片中丹参酮ⅡA和丹酚酸B的含量测定方法.     

HPLC法测定脑通颗粒中丹酚酸B

目的 建立HPLC法测定脑通颗粒中丹酚酸B.方法 采用迪马色谱柱(250 mm×4.6 mm,5 μm);以甲醇-乙腈-甲酸-水溶液(30:10:0.5:59.5)为流动相;检测波长286 nm;体积流量1.0 mL/min:柱温40℃;进样量10μL.结果 丹酚酸B在0.441 6～2.208 0 μg线性关系良好(...     

高效液相色谱法测定肾复康胶囊中丹酚酸B的含量

目的采用高效液相色谱法测定肾复康胶囊中丹酚酸B的含量。方法采用Agilent Zorbax SB C_(18)(4.6 mm×250 mm,5μm)色谱柱,乙腈-0.2%磷酸溶液(24∶76)为流动相,流速为1.0 mL/min,检测波长为286 nm,柱温为25℃,进样量10μL,运行时间为20 min。结果丹酚酸B在5.00~100μg/m L范围线性关系良好,r=0.999 6(n=6),平均回收率为100.3%,RSD=0.85%。结论本方法简便、准确,灵敏度高,重现性良好,可用于肾复康胶囊中丹酚酸B的质量控制。     

HPLC法测定参梅养胃颗粒中丹酚酸B的含量

目的:建立HPLC法测定参梅养胃颗粒中丹酚酸B的含量.方法:采用Agilent TC-C18柱(4.6mm×150mm,5μm),以甲醇-乙腈-甲酸-水(30:10:1:59)为流动相,流速1.0mL/min,检测波长286nm,柱温30℃.结果:丹酚酸B的浓度在0.0082~0.0409mg/mL范围内线性关系良好(r=0.9992,n=5),平均加样回收率为101.0%,RSD%为1.8%(n=6).结论:该方法测定结果稳定,重复性好,灵敏度高,操作简便,可以作为测定丹酚酸B含量的方法.     

HPLC-DAD同时测定心舒宝片中3种成分的含量

目的 建立心舒宝片中没食子酸、芍药苷、丹酚酸B 3种成分的HPLC含量测定方法,为心舒宝片的质量控制提供参考.方法 采用HPLC-DAD法,岛津ODS C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.15％磷酸水溶液梯度洗脱,检测波长230 nm(芍药苷)和286 nm(没食子酸、丹酚酸B),柱温...     

HPLC法同时测定活络消痛片中紫丁香苷、阿魏酸和丹酚酸B含量

目的:建立HPLC法同时测定活络消痛片中紫丁香苷、阿魏酸和丹酚酸B的含量。方法:色谱柱为Kromasil C18柱(150 mm×4.6 mm,5μm),流动相为甲醇-0.2%磷酸溶液,梯度洗脱,流速为1.0 ml·min-1,检测波长为紫丁香苷(265 nm),阿魏酸(321 nm),丹酚酸B(286 nm),柱温为25℃。结果:紫丁香苷、阿魏酸和丹酚酸B分别在64.500~1.032×103μg·ml-1、7.525~120.400μg·ml-1、65.250~1.044×103μg·ml-1范围内与峰面积呈良好的线性关系,平均回收率分别为100.75%、99.56%、99.75%。结论:本方法简便、准确、快速。     

HPLC测定大红袍妇炎宁胶囊中的丹参酮ⅡA和丹酚酸B

目的建立测定大红袍妇炎宁胶囊中丹参酮ⅡA和丹酚酸B的方法。方法采用RP-HPLC法,Eclipse-XDB-C18(150 mm×4.6 mm,5μm)色谱柱,测定丹参酮ⅡA的流动相为甲醇-水(75:25),检测波长270 nm;测定丹酚酸B的流动相为乙腈-甲醇-1.7%甲酸(10:25:65),检测波长310 nm。结果丹参酮ⅡA3.38~30.42μg.ml-1与峰面积呈线性关系(r=0.9999);丹酚酸B 12.9~116.1μg.ml-1与峰面积呈线性关系(r=0.9998),丹参酮ⅡA的平均回收率为100.9%,RSD=1.31%(n=9);丹酚酸B的平均回收率为100.8%,RSD=1.27%(n=6)。结论所建方法简便、准确、可靠,可用于大红袍妇炎宁胶囊中丹参酮ⅡA和丹酚酸B的含量测定。     

芪参健骨颗粒中丹酚酸B的含量测定方法分析

目的构建测定芪参健骨颗粒中丹酚酸B含量的方法。方法选择HPLC法,色谱柱为5μm,4.5mm×150mm的SB-C18柱,1mol/L的水∶甲酸∶乙腈∶甲醇的流动相,比例为62∶2∶7∶26。0.9mL/min的流速,243mm的检测波长,25℃的柱温。结果在0.1295～2.590μg/mL的范围内,丹酚酸B含量的线性关系呈现良好,r=0.9996,回收率平均值为99.5%,RSD=1.2%。结论测定丹酚酸B含量,采用高效液相色谱法,较为简单、快捷,测定结果可靠。     

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.     

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.     

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.