毛细管气相色谱法检测水皂角等中药提取物有机氯农药残留

目的:建立水皂角等中药提取物中六六六及滴滴涕异构体含量的气相色谱分析方法。方法:样品采用改进了的微量化学法进行提取,浓硫酸净化,以不分流方式进样,用HP-5弹性石英毛细管柱分离样品,微电子捕获检测器检测,载气为高纯氮气,流速为1.5 mL·min-1,尾吹速度为40 mL·min-1,进样口温度250℃,检测器温度300℃。柱初始温度为100℃,以20℃·min-1升至160℃后,保持2 min,以10℃·min-1升至250℃,保持6 min。结果:最小检测量为1.4×10-14-1.2×10-12g,加样平均回收率为93.2％-101.6％;被测样品中均含有不同程度的有机氯农药残留。结论:该法快速、灵敏、准确,各项技术指标均满足农药残留检测的要求。     

气相色谱法测定紫金散中麝香酮的含量

目的:建立紫金散中麝香酮含量测定方法。方法:硝基对苯二甲酸改性聚乙二醇毛细管柱(HP-FFAP)(柱长为25 m,柱内径为0.2 mm,膜厚度为0.3μm),柱温为程序升温,初始温度120℃,保持1 min,以8℃.min-1的速率升至190℃,保持5min,再以40℃.min的速率升至240℃,保持10 min;进样口温度230℃,检测器温度250℃,分流比3.0∶1,进样量1μL。结果:麝香酮在7.12~0.142 4 mg.L-1范围内呈良好的线性关系。平均回收率为97.1%(RSD=2.1%)。结论:本方法简便、快速、准确,可用于控制紫金散中人工麝香的含量。     

GC法测定万金油中桉油精和丁香酚的含量

目的:建立万金油中桉油精和丁香酚的含量测定方法。方法:采用气相色谱法。色谱柱为HP-FFAP,固定相为交联聚乙二醇-TPA;氢火焰离子化检测器,进样口温度:230℃,检测器温度:250℃;分流进样,分流比:20∶1;程序升温:初始80℃,保持3min,以6℃·min-1升至200℃,保持7min;载气:氮气,流速:1.0mL·min-1。结果:桉油精和丁香酚检测浓度线性范围分别为0.091～1.174(r=0.9999)、0.014～0.174mg·mL-1(r=0.9981),平均回收率分别为100.49%(RSD=1.47%,n=6)和100.01%(RSD=1.82%,n=6)。结论:该方法简便、快速、准确,可用于万金油的质量控制。     

GC法同时测定蜂房药材中5个脂肪酸的含量

目的:建立衍生化气相色谱法同时测定蜂房药材中脂肪酸类含量的方法,比较不同产地的蜂房中5个脂肪酸的含量。方法:采用AB-INOWAX毛细管色谱柱(30 m×0.25 mm,0.25μm);程序升温,起始温度150℃,以5℃·min-1速率升至190℃,保持2 min;再以5℃·min-1速率升至240℃,保持9 min。进样口温度250℃;FID检测器,检测器温度250℃;载气为氮气,流速1.83 m L·min-1;分流比为80∶1。结果:棕榈酸甲酯、硬脂酸甲酯、油酸甲酯、亚油酸甲酯、α-亚麻酸甲酯质量浓度分别在0.08~0.77、0.02~0.23、0.17~2.70、0.11~1.12、0.08~0.82 mg·m L-1范围内呈现良好的线性关系,相关系数分别为0.999 9、0.999 7、0.999 3、0.999 8、0.999 8;平均回收率(n=6)分别为102.4%、103.3%、98.0%、100.2%、97.7%,RSD均≤2.5%。按脂肪酸甲酯标准曲线计算,并换算为脂肪酸含量,12批样品中棕榈酸、硬脂酸、油酸、亚油酸、α-亚麻酸的含量测定结果分别为1.42~24.79、0.48~2.72、1.89~34.48、0.78~4.81、1.26~19.55 mg·g-1。结论:该方法可作为蜂房中脂肪酸的含量测定及鉴别方法。     

气相色谱法测定保济丸中百秋李醇的含量

目的:建立以气相色谱法测定保济丸中百秋李醇含量的方法,制定并完善保济丸的质量标准。方法:采用非极性毛细管柱AT.SE-54(15m×0.25mm×0.33μm),柱温采用程序升温:起始150℃,保持23min,以8℃·min-1速率升至230℃,保持2min,进样口温度为280℃,检测器(FID)温度为280℃,载气为氮气,流速为1.0mL·min-1。结果:百秋李醇进样量在0.12～0.36μg范围内线性关系良好(r=0.9999),平均加样回收率为98.62%,RSD=4.69%。结论:该方法稳定、结果可靠、重复性好,可作为保济丸质量控制标准之一。     

气相色谱法测定柴荆注射液中正己酸和胡薄荷酮含量的研究

目的:测定柴荆注射液中正己酸和胡薄荷酮的含量以控制产品质量。方法:采用HP-50+石英毛细管柱(相当于OV-17),以苯甲醇为内标物,程序升温:初始温度60℃,保持6 min,然后以5℃·min~(-1)升温至110℃,保持3 min,再以30℃·min~(-1)升温至250℃,保持25 min。汽化室温度:260℃;检测器:FID检测器;检测器温度:280℃;载气:氮气。结果:正己酸及胡薄荷酮线性范围分别为0.018～0.09 mg·mL~(-1)(r=0.9997)和0.022～0.11mg·mL~(-1)(r=0.999 7),精密度实验的RSD(n=5)均为4.8％,重复性实验的RSD(n=5)分别为1.0％和4.0％,平均回收率(n=5)分别为98.6％(RSD=4.9％)和104.4％(RSD=4.3％)。结论:该方法准确、重现性好、简便、易行,可用于质量控制。     

感冒清热颗粒挥发油特征图谱及薄荷酮和胡薄荷酮的含量测定

目的:建立感冒清热颗粒中挥发油的特征图谱并测定其中薄荷酮和胡薄荷酮的含量。方法:Agilent HP-5毛细管柱(30 m×320 mm,0.25μm);进样口、检测器温度250℃;柱温:初始温度40℃,保持1 min,7℃.min-1升至100℃,保持12min,3℃.min-1升至150℃,保持8 min,10℃.min-1升至240℃,保持2 min;载气为氮气;流速:1 mL.min-1;不分流。结果:特征图谱中标定了6个共有峰。薄荷酮进样量在0.0211～0.422μg,胡薄荷酮进样量在0.0371～0.743μg内均呈良好的线性关系(r=0.9999);平均回收率分别为101.0%和97.5%,RSD均小于3%。结论:建立的气相色谱特征图谱及含量测定方法可从定性和定量两方面控制感冒清热颗粒中的挥发性成分,方法准确、可行,可作为感冒清热颗粒的质量控制方法。     

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。     

GC-MS/MS测定头孢拉定原料中N,N-二甲基甲酰胺及N-甲基乙酰胺的残留量

摘要：目的:建立GC-MS/MS测定头孢拉定原料中N,N-二甲基甲酰胺（DMF）及N-甲基乙酰胺（NMAC）的残留量的方法。方法:色谱条件Agilent VF-WAXms毛细管柱（30 m×0.25 mm, 0.25μm）,进样口温度为250℃;载气为高纯氦气,进样口为恒流模式,流速1.0 ml·min-1;分流进样,分流比10∶1。程序升温:初始温度50℃,保持1min,以10℃·min-1的速率升至180℃,保持2 min,再以20℃·min-1的速率升至240℃,保持10 min。质谱条件离子源为电子轰击源（EI）,离子源温度280℃。碰撞气为氮气,流速1.5 ml·min-1。质谱传输接口温度250℃。质谱监测模式为多反应监测（MRM）。结果:DMF在0.109～7.270μg·ml-1内与其峰面积呈良好的线性关系（r=0.999 9）,加标回收率为92.70%（RSD=4.28%,n=6）;NMAC在0.109～7.280μg·ml-1内与其峰面积呈良好的线性关系（r=0.999 9）,加标回收率为109.89%（RSD=4.24%,n=6）。结论:本方法经方法学验证,可用于测定头孢拉定中DMF及NMAC的残留量。     

HPLC法测定魟鱼鱼油中二十碳五烯酸、二十二碳六烯酸的含量

目的:建立魟鱼鱼油中二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)的含量测定方法。方法:色谱柱为Diamonsil C18,流动相为乙腈-水(95∶5),流速为1.0mL·min-1,检测波长为220nm,柱温为25℃。结果:EPA和DHA进样量检测线性范围分别为1～4μg、2～8μg(rEPA=0.9991,rDHA=0.9994),平均加样回收率分别为99.23%、99.30%,RSD分别为0.49%、0.27%。结论:本方法简便、快速、稳定、重复性好,可用于魟鱼鱼油中EPA、DHA的鉴别和含量测定。     

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.