GC法测定复方苦参注射液中聚山梨酯80的含量

目的:建立测定复方苦参注射液中聚山梨酯80含量的气相色谱方法。方法:采用脂肪酸甲酯化法进行样品前处理。气相色谱条件:DB-WAX毛细管柱(PEG-20000,30 m×0.32 m×0.25 m);氢火焰离子化检测器(FID);进样口温度250℃,检测器温度为250℃;柱温初始温度为80℃,以10℃.min-1升温至220℃,保持20 min;载气为氮气,恒定流速1 mL.min-1,进样方式为分流进样,分流比10∶1;进样量为1μL。结果:聚山梨酯80的进样浓度在0.1～5.0 mg.mL-1(r=0.9998)范围内呈良好线性关系;平均回收率(n=3)为97.4%～100.7%。结论:该方法简便快速,可用于复方苦参注射液中聚山梨酯80的含量测定。     

盐酸头孢吡肟中残留溶剂N,N-二甲基甲酰胺的检测方法

目的 建立顶空气相色谱法测定盐酸头孢吡肟中残留溶剂N,N-二甲基甲酰胺的含量的方法.方法 色谱柱为DB-624毛细管柱(30m×0.53m,3μm),柱温:程序升温,90℃维持18min,以每分钟20℃升温至200℃,维持5min;检测器温度为250℃;进样口温度为200℃,分流比1:1.顶空进样,项空瓶平衡温度为90℃,平衡时间为40min,进样体积为1.0mL.结果 N,N-二甲基甲酰胺在0.0290mg·mL-1～0.2 07mg·mL-1浓度范围内线性关系良好(r值为0.99975),平均回收率为101.1%(RSD为1.7%).结论 该方法准确灵敏,可用于盐酸头孢吡肟中二甲基甲酰胺的检测.     

毛细管气相色谱法测定盐酸美金刚原料药中三氯甲烷的残留量

目的:建立毛细管气相色谱法测定盐酸美金刚原料药中三氯甲烷残留量的方法。方法:色谱柱为DB-1701石英毛细管柱,柱温采用程序升温,检测器为电子捕获检测器,检测器温度为250℃,进样口温度为200℃,以N,N-二甲基甲酰胺为溶剂。结果:三氯甲烷检测浓度线性范围为1.2～60μg·mL-(1r=0.9999);平均回收率为99.6%(RSD=0.8%);定量限为1.02pg;3批样品中三氯甲烷残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于盐酸美金刚原料药中三氯甲烷残留量的测定。     

气相色谱法测定止痒消炎水中薄荷脑、冰片和麝香草酚的含量

目的建立同时测定止痒消炎水中薄荷脑、冰片和麝香草酚含量的气相色谱测定方法。方法采用气相色谱内标法,FID检测器,HP-INNDW AX石英毛细管柱(30m×250μm,0.25μm),应用程序升温(140℃保持4.1min以后20℃.min-1升至240℃),进样口温度200℃,检测器温度250℃;分流进样,分流比10:1。结果薄荷脑在0.32～3.2mg.mL-1,冰片在0.56～5.6mg.mL-1,麝香草酚在0.16～1.6mg.mL-1内呈良好的线性关系,加样回收率,薄荷脑为99.8%,(RSD=1.3%);冰片为99.2%(RSD=1.5%);麝香草酚为99.8%(RSD=0.9%)。结论该方法简单可靠,适合于止痒消炎水中薄荷脑、冰片和麝香草酚的含量测定。     

气相色谱法同时测定无极膏中5个挥发性有效成分的含量

目的:建立同时测定无极膏中合成樟脑、薄荷脑、水杨酸甲酯、冰片和麝香草酚5种主要成分含量的分析方法。方法:采用气相色谱法,色谱柱为聚乙二醇(PEG)-20M毛细管色谱柱(30 m×0.32 mm×0.25μm),检测器为FID检测器,进样口温度为250℃,检测器温度为250℃。升温程序为初始温度150℃,保持5 min;10℃.min-1升温至200℃,保持8 min;再以20℃.min-1升温至240℃,保持25 min,分流比为10∶1。结果:合成樟脑、薄荷脑、水杨酸甲酯、冰片和麝香草酚浓度分别在1.4934～7.4672 mg.mL-1(r=0.9999),0.9304～4.6520 mg.mL-1(r=0.9999),0.9075～4.5376 mg.mL-1(r=0.9999),0.1387～0.6936 mg.mL-1(r=0.9999),0.0716～0.3580 mg.mL-1(r=0.9999)质量浓度范围内线性关系良好。平均回收率(n=9)分别为98.8%,99.4%,98.6%,99.6%,99.7%。结论:该方法灵敏、快速简便、准确,可有效地控制无极膏的质量。     

GC法测定蛇脂冰肤软膏中薄荷脑和冰片的含量

目的:采用气相色谱法测定蛇脂冰肤软膏中薄荷脑、冰片的含量。方法:样品经正己烷超声处理后,采用Agilent INNO-WAX毛细管色谱柱(30 m×0.25 mm×0.25μm);FID检测器;色谱条件:柱温:110℃,载气流速1.5 mL.min-1,进样口温度:250℃,检测器温度:300℃。进样量:1μL。结果:薄荷脑在0.0762～6.0995 mg.mL-1范围内线性关系良好(r=0.9999,n=6),龙脑在0.0460375～3.683 mg.mL-1范围内线性关系良好(r=0.9999,n=6)。薄荷脑的平均加样回收率(n=9)为101.1%,龙脑的平均加样回收率(n=9)为101.7%。结论:该方法灵敏度高、专属性好、操作简便、重现性好。     

GC同时测定麝香通心滴丸中龙脑、异龙脑和麝香酮的含量

摘要：目的 建立同时测定麝香通心滴丸中龙脑、异龙脑及麝香酮含量的气相色谱法。方法 色谱柱：HP-5MS毛细管色谱柱(30 m×0.32 mm,0.25 μm),检测器为FID检测器,检测器温度为250 ℃,进样口温度220 ℃。柱温以100 ℃为初始温度,保持2分钟,以2 ℃?min-1升温至110 ℃,保持3分钟,以50 ℃?min-1升温至205 ℃,保持7分钟,以20 ℃?min-1升温至250 ℃,保持2分钟;载气为氮气,流速为1 mL?min-1;进样方式为分流进样,分流比为10：1;进样量为1 μL,以萘为内标。结果 龙脑、异龙脑、麝香酮的浓度分别在0.05468~0.4374 mg?mL-1(r=0.9999),0.07067~0.5654 mg?mL-1(r=0.9999),0.004512~0.03610 mg?mL-1(r=0.9997)的范围内线性良好;平均回收率分别为97.91 %(RSD=2.05 %),100.79 %(RSD= 2.78 %),105.36 %(RSD=3.78 %)。结论 该方法有效可靠,可用于麝香通心滴丸中龙脑、异龙脑和麝香酮的含量测定。     

气相色谱-电子捕获检测器法测定异氟烷的含量

目的:建立测定异氟烷含量的方法。方法:采用气相色谱-电子捕获检测器法。色谱柱为HP-INNOWax毛细管柱,柱温为75℃,检测器为ECD检测器,检测器温度为250℃,分流比为1:1,进样口温度为150℃,载气为氮气,流速为5mL.min-1,进样量为1μL。结果:异氟烷检测浓度在0.1002～1.201mg.mL-1范围内与峰面积积分值线性关系良好(r=0.9999);平均回收率为99.90%～100.00%,RSD=0.10%(n=9)。结论:该方法灵敏度高,重复性好,结果准确、可靠,适用于异氟烷的含量测定。     

气相色谱法测定盐酸美金刚缓释胶囊的含量

目的建立气相色谱法测定盐酸美金刚缓释胶囊含量的分析方法。方法采用气相色谱法,DB-1石英毛细管柱(30m×0.53mm,1.0μm),进样口温度为210℃;氢火焰离子化(FID)检测器,载气为氮气,检测器温度为300℃,柱初温70℃,以5℃/min升温速率升至170℃;以盐酸金刚烷胺为内标物测定盐酸美金刚缓释胶囊的含量。结果盐酸美金刚在28.4~568μg/m L范围线性关系良好,相关系数大于r=0.9990(n=6),精密度试验的RSD为小于0.49%(n=6)。结论所建立的方法准确、回收率较为理想,能满足盐酸美金刚缓释胶囊的含量测定。     

顶空气相色谱法测定灯盏花滴丸中残留溶剂

目的:建立灯盏花滴丸中乙醇、正丁醇残留量的测定方法。方法:采用DB-624毛细管色谱柱(30 m×0.32 mm,1.80μm),载气为氮气,流速为1.0 mL.min-1,柱温90℃;顶空进样,进样口温度200℃;氢火焰离子化检测器(FID),检测器温度250℃。结果:乙醇和正丁醇线性范围分别为0.0201～1.0067 mg.mL-1(r=0.9998)和0.0200～1.0020 mg.mL-1(r=0.9998),平均回收率(n=9)分别为101.1%和105.1%。结论:该方法简便,灵敏度高,重复性好,结果准确,适合灯盏花滴丸中有机溶剂残留量的测定。     

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.