党参饮片中党参内酯和党参炔苷的相关性研究

目的：分析不同来源党参饮片中党参内酯和党参炔苷的含量，对实验结果进行比较，找出其相关性，更好地控制党参的质量。方法：采用反相高效液相色谱法分析，色谱柱：C18（250mm×4．6mm，5μm）．以乙腈-水（70：30）为流动相，测定党参内酯的含量，检测波长为220nm；以乙腈-0．1％HAc（26：74）为流动相，测定党参炔苷的含量，检测波长为267nm。结果：在选定的色谱条件下，这2种活性成分的分离度良好，党参内酯的回归方程为Y=4．01×10^6X＋6．95×10^2，r=0．9997，平均回收率为99．9％，RSD为1．9％（n=6），线性范围为0．01～0．10μg；党参炔苷的回归方程为Y=8．51×10^5X＋1．67×10^4，r=0．9990，平均回收率为99．9％，RSD为1．0％（n=6），线性范围为0．05～0．25μg。所测样品中2种成分的含量基本在12个样品中呈相同的顺序排列。结论：党参内酯和党参炔苷含量之间有一定的相关性，这为简便快速控制党参的质量提供了依据。     

高效液相色谱法测定排石利胆颗粒中龙胆苦苷的含量

目的：建立排石利胆颗粒中龙胆苦苷的含量测定方法。方法：选用Kromasil C128色谱柱（250mm×4．6mm，5μm）；以甲醇-水（22：78）为流动相；检测波长270nm，流速1．0ml·min-1。结果：线性范围是0．106～0．950μg（r=0．9998），平均回收率98．8％，RSD1.3％。结论：此方法简便，快速，准确，可用于排石利胆颗粒中龙胆苦苷的含量测定。     

高效液相色谱-蒸发光散射检测法测定安心康滴丸中黄苠甲苷的含量

目的：建立安心康滴丸中黄芪甲苷的高效液相测定方法。方法：采用高效液相-蒸发光散射检测法测定黄芪甲苷的含量。色谱柱为AgilentC18柱（250mm×4．6mm，5μm），以乙腈-水（38：62）为流动相，柱温为室温，流速为1.0mL·min^-1。ELSD参数为：漂移管温度为55℃，氮气压力为2．5×10^5Pa。结果：黄芪甲苷在0．5-10μg范围内与峰面积有良好的线性关系（r=0.9997），平均回收率为97．7％（RSD为1．49％）。结论：该方法精密度高，重复性好，可用于测定黄芪甲苷的含量。     

高效液相色谱法测定格列本脲片和格列齐特片的含量

目的建立HPLC法同时测定格列本脲片、格列齐特片的含量。方法采用HPLC法测定，Phenomenex C18（250mm×4．6mm，5μm）柱，柱温25℃；流动相为0．025mol·L^-1磷酸二氢钾溶液（用磷酸调节pH值至3．4）-甲醇（3：7）；流速为1．0mL·min^-1；检测波长为230nm。分别以外标法计算含量。结果格列本脲在0．016-0．403mg·mL^-1线性关系良好，回归方程Y=3×10^7X＋1．37×10^5，r=0．9996。平均回收率为98．44％，RSD=0．41％。检测限低于1．61ng，格列齐特在0．015-0．382mg·mL^-1线性关系良好，回归方程Y=2×10^7X＋1．00×10^5，r=0．9996。平均回收率为97．97％，RSD=1．70％。检测限1．52ng。结论本方法可同时测定格列本脲片、格列齐特片的含量，灵敏度高、操作简便、准确可靠。     

HPLC法测定金胆片中龙胆苦苷、虎杖苷含量

目的：建立测定金胆片中龙胆苦苷、虎杖苷含量的HPLC法,分析151批金胆片质量,为金胆片质量标准的统一、完善提供依据。方法：色谱柱：Diamonsil C18（250mm×4．60mm,5μm）;流动相：甲醇-水,梯度洗脱;检测波长：288nm;柱温：30℃;进样量10μl。结果：龙胆苦苷线性范围：5～100μg·ml^-1（r=0．9999）,平均加样回收率为99．4％,RSD为1．4％（n=6）;虎杖苷线性范围：4～80μg·ml^-1（r=0．9998）,平均加样回收率为100．4％,RSD为1．3％（n=6）。结论：该方法简便,快速,准确,可用于测定金胆片中龙胆苦苷、虎杖苷的含量。不同厂家生产的金胆片中龙胆苦苷、虎杖苷的含量差异较大。     

HPLC法测定西多福韦的含量及有关物质

目的：建立测定西多福韦的含量及有关物质的高效液相色谱法。方法：采用Platisil ODS色谱柱（250mm×4．6mm，5μm），流动相：甲醇-磷酸盐缓冲液（每1L含25mmol磷酸二氢钠，25mmol磷酸氢二钠，pH=6．8）（2：98），流速为1．0mL·min^-1，检测波长274nm，柱温25℃。结果：西多福韦的浓度在0．0408～163．2μg·mL^-1。范围内线性良好（A=3．4×10^4C＋1．8×10^4，r=0．9999）；方法的最低检测限为0．163ng（S／N=3）；高、中、低3种浓度的加样回收率（n=3）分别为99．9％（RSD=0．23％），100．0％（RSD=0．00％），99．9％（RSD=0．17％）；日内精密度RSD=0．18％（n=6）；各杂质峰与主峰达到基线分离。结论：此法操作简便、灵敏、准确，重复性好，适用于西多福韦的含量及有关物质的测定。     

RP-HPLC法测定甲硝唑栓的含量

目的建立高效液相色谱法来检测甲硝唑栓的含量。方法采用色谱柱：Thermo C18（250mm×4．6mm，5μm）；流动相：甲醇-50mmol·L^-1。磷酸二氢钾溶液（20：80），流速：1．0ml·min。；柱温30℃； 检测波长：310nm；进样量：20μl。结果本研究建立的检测方法能在该色谱条件下把甲硝唑与其辅料完全分离开来，回归方程分别为：A=3．47×10^4C-0．88×10^4，r=0．9999（n=3），回收率为98．4％，RSD为0．9％。结论该检测技术具有快速、简便、灵敏、重复性好、便于操作、专属性强等优点。     

HPLC—MS测定十味龙胆花颗粒中的龙胆苦苷和小檗碱

目的：建立一种快速灵敏的同时测定十味龙胆花颗粒中的有效成分龙胆苦苷和小檗碱的HPLC—MS方法。方法：样品用50％甲醇溶液超声提取，采用Zorbax SBC18（4．6mm×250mm，5μm）色谱柱，以含0．2mmol·L^-1醋酸钠的1％醋酸水溶液（A）-甲醇（B）为流动相进行梯度洗脱（0～10min，33％B；19min，60％B；19．01min，80％B），流速0．8mL·min^-1；在ESI正离子模式下，采用选择性离子监测方法（0—14min，m／z 379；14～22min，m／z 336）。结果：龙胆苦苷、小檗碱的线性范围分别为0．030～30．0μg·mL^1（r=0．9992）和0．004～10．0μg·mL^-1（r=0．9990），检出限分别为0．010μg·mL^-1和0．0013μg·mL^-1样品加样回收率为99．2％～103．3％，日内、日间精密度试验的RSD均低于5％。结论：方法快捷、准确，重复性好，可用于药品十味龙胆花颗粒的分析。     

HPLC法测定龙胆中龙胆苦苷的含量

目的：采用HPLC法测定（Agilent Eclipse XDB—C18柱,150mm×4．6mm,5um）龙胆中龙胆苦苷的含量。方法采用高效液相色谱法;C18色谱柱（流动相：甲醇-水（25：75）流速：1ml／min;检测波长：270nm;柱温：25℃;进样量：10ul。结果：龙胆苦苷在0．1mg／mL-1．0mg／mL之间线性良好。得回归方程,Y=309．72X-16．788,r=0．9998。,测得龙胆苦苷平均加样回收率为99．38％。KSD为0．62％。结论：本法快速简便,准确,重现性好。     

除湿注射液中龙胆苦苷和苦参碱的HPLC测定

建立了HPLC法测定除湿注射液中龙胆苦苷和苦参碱的含量。采用Diamondial C18柱，流动相为乙腈-甲醇-水-三乙胺（4：23：73：0．45，磷酸调至pH6．8），检测波长215nm。龙胆苦苷和苦参碱在3．125～100μg／m1范围内线性关系良好，回收率大于98％，日内、日间RSD均小于2％。     

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.