五种常用大孔树脂残留物的比较

目的:建立用气相色谱法检测大孔吸附树脂中正己烷、苯、甲苯、二甲苯和苯乙烯五种有机残留物的方法。方法:采用毛细管气相色谱法,色谱柱为DB-624毛细管色谱柱;进样口温度为200℃,FID检测器温度240℃,柱温为程序升温:柱起始温度为40℃,保持3 min,然后以每分钟14℃的速率升至200℃,保持2 min。甲醇为溶解介质,载气为氮气,测定常用大孔树脂正己烷、苯、甲苯、二甲苯和苯乙烯五种有机残留物。结果:五种常用大孔树脂D101、HPD100、AB-8、DM301、NKA-9中正己烷、苯、甲苯、二甲苯、苯乙烯含量均小于20‰。符合国家相关规定。结论:该方法简便易行、重复性好,可控制大孔树脂有机溶剂残留量。     

药用胶塞中正己烷的含量测定及迁移研究

目的建立测定药用胶塞中正己烷含量的气相色谱法。方法采用气相色谱法测定氯化丁基胶塞中正己烷的含量及在包装药品中的迁移情况。色谱柱为DB-624毛细管柱(30 m×0.320 mm,1.80μm);FID检测器,温度为280℃;载气为N2;柱流量为2.0 mL/min;柱温采用程序升温,45℃保持7 min,8℃/min升至110℃保持7 min,60℃/min升至250℃保持3 min;进样口温度为280℃,分流比为20∶1,进样量为1μL。结果正己烷质量浓度在0.5~50μg/mL范围内与峰面积线性关系良好(R2=1),在19 h内稳定性良好,检出限为0.22μg/mL,平均加样回收率为95.75%(n=9);氯化丁基胶塞中正己烷含量为1.51μg/g,迁移药品中均未检出正己烷。结论该方法操作简单、结果准确、灵敏度高、重复性好,可用于药用胶塞中正己烷的含量测定。     

气相色谱法测定西黄胶囊中麝香酮的含量

目的建立测定西黄胶囊中麝香酮的气相色谱法。方法色谱柱:OV-17毛细管柱(30.0m×0.32mm,1.0μm);初始柱温:150℃,保持26min;再以20℃.min-1的升温速率升至230℃,保持20min;进样口温度:200℃;检测器温度:250℃;载气:氮气;流速:2.0mL.min-1。结果回归方程线性关系良好,线性范围为1.5～299.2mg.L-1,平均回收率为94.7%,RSD1.3%。结论该方法准确、灵敏,能有效控制西黄胶囊的质量。     

NP-HPLC法测定人血浆中劳拉西泮的浓度

目的:建立检测人血浆中劳拉西泮浓度的正相高效液相色谱方法.方法:血浆样品用乙醚萃取,55℃水浴中氮气吹干;残留物用无水乙醇溶解后进样.色谱柱为Shim-pack CLC-CN柱(150mm×6.0mm,5μm),流动相为正己烷-甲醇-无水乙醇(79︰17.3︰3.7),流速为1.15ml·min-1,柱温为:30℃,紫外检测波长为230nm.结果:劳拉西泮浓度在0.01～2.0μg·ml-1内线性关系良好(r=0.9996);日内、日间RSD均小于4.7%(n=6).结论:本方法灵敏,特异性强,准确,简便易行,适用于劳拉西泮血浓度的临床监测和药代动力学研究.     

不同产地苍艾挥发油的GC-MS指纹图谱研究

目的:建立苍艾挥发油的气相色谱-质谱(GC-MS)指纹图谱,分析苍艾挥发油的化学组成,为其质量控制提供方法和依据.方法:Agilent DB-5MS石英毛细管色谱柱(30m×0.25mm×0.25μm),柱温40℃(保持1 min),以10℃·min-1速率升至130℃(保持5 min),以8℃·min-1速率升至25...     

姜三七挥发油指纹图谱研究

目的建立姜三七挥发油气相色谱指纹图谱。方法采用水蒸汽蒸馏法提取挥发油,色谱柱为DB-1701（30m×0.25μm×0.32 mm）毛细管柱,检测器为FID检测器,采用程序升温,柱温110℃,保持5 min,以4℃min-1的升温速率升至160℃,保持3 min;再以2℃min-1的升温速率升至180℃,保持3 min;最后以3℃min-1的升温速率升至240℃,保持3 min。结果依据11批药材的指纹图谱数据建立共有模式,得到共有峰10个。结论本测定方法为姜三七药材的质量评价提供了科学依据。     

GC-MS法测定荆芥挥发油中薄荷酮、胡薄荷酮含量

采用气相色谱-质谱联用法,选用毛细管气相色谱柱H-5MS(5%henyl Methyl Silox-ane,30.0 m×250.0μm×0.25μm),程序升温方法:初始温度50℃,以10℃.min-1速率升至100℃,保持10min,再以5℃.min-1速率升至200℃,保持5min。薄荷酮在0.00517～0.1034mg.mL-1之间呈良好的线性关系(r=0.9999);胡薄荷酮在0.0372～0.744mg.mL-1之间呈良好的线性关系(r=0.9991)。薄荷酮回收率为98.0%,RSD(%)=1.696;胡薄荷酮回收率为99.4%,RSD(%)=2.469。     

毛细管气相色谱法测定舒必利中有机溶剂残留量

目的：建立气相色谱法测定舒必利中3种有机溶剂的残留量的方法.方法：采用HP-1毛细管色谱柱（30.0 m×0.53 mm,5μm）;进样口温度为205℃;FID检测器温度为280℃;柱温：程序升温,60℃保持5 min,然后以20℃·min-1的速率升温120℃,保持5 min;以氮气为载气,载气流速为3.0 ml· min-1;直接进样,进样量为1μl;以N,N-二甲基甲酰胺为溶剂.结果：甲醇,乙醇和乙二醇及溶剂峰彼此均能良好分离,线性范围分别为1.51 ～ 301.72 μg·ml-1（r =0.999 9）,1.51 ～ 502.56μg·ml-1（r =0.999 9）,4.11～65.76 μg·ml-1（r =0.999 1）;平均回收率分别为93.6％,91.7％,92.8％,RSD分别为2.5％,3.0％,5.7％（n=9）.结论：该法准确可靠,适用于舒必利中这3种有机溶剂残留量的测定.     

RP-HPLC法测定百乐眠胶囊中大黄素和大黄素甲醚的含量

目的建立RP-HPLC法测定百乐眠胶囊中大黄素和大黄素甲醚的含量。方法采用lichrospher C18色谱柱,流动相为甲醇：0.1%磷酸水溶液（82∶18）,流速为：1.0mL·min^-1,检测波长：254nm,柱温35℃。结果大黄素在0.0392～0.2741μg,r=0.9999,大黄素甲醚在0.0506～0.3544μg线性关系良好,r=0.9999。平均回收率大黄素为100.54%（RSD=2.18%）、大黄素甲醚为102.63%（RSD=1.63%）。结论本方法操作可靠、准确,适用于百乐眠胶囊中大黄素和大黄素甲醚的含量测定。     

顶空-气相色谱法测定药酒中的甲醇量

目的建立药酒中甲醇量的测定方法。方法采用顶空-气相色谱法,色谱柱为Agilent Technologies DB-WAX(30m×0.32mm×0.25μm),FID检测器;进样口温度:140℃;检测器温度220℃;载气流速:0.3 mL·min-1;梯度升温:29℃保持1min,以0.5℃·min-1速率升至31℃,保持10min,以5℃·min-1速率升至65℃,保持1 min,以50℃·min-1速率升至200℃,保持2min;时间周期:38min。结果甲醇在0.000 1~0.005mL·mL-1范围内线性关系良好,r=0.999 4,平均回收率为99.6%,RSD 2.5%(n=6)。结论该方法检测结果准确、专属性强、灵敏度高、重复性好,可用于药酒中甲醇量的控制。     

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.

     

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.