高效毛细管电泳法测定育亨宾树皮中育亨宾的含量

目的建立高效毛细管电泳(HPCE)测定育亨宾树皮中育亨宾含量的方法。方法运用高效毛细管电泳方法,熔融石英毛细管(75μmID×50cm),缓冲液为20mmol·L-1磷酸盐缓冲液(PH=3.0),检测波长:270nm,分离电压:15kV,柱温25℃,用0.45μm微孔滤膜过滤后进样,压力进样:50mbar×5s。结果方法最低检测浓度为0.1μg·mL-1,线性范围1～200μg·mL-1,r=0.9991,线性关系良好。精密度RSD为1.3%,回收率为98.4%。结论本法简单、灵敏经济,可作为育亨宾树皮中育亨宾的含量的测定。     

高效毛细管电泳法测定头孢克洛干混悬剂中头孢克洛的含量

目的:测定头孢克洛干混悬剂中头孢克洛的含量.方法:采用高效毛细管电泳法.毛细管柱(60cm×75μm),运行缓冲液30mmol·L-1硼砂(pH 9.2),高压进样5s,分离电压12kV,温度为25℃,检测波长为254nm,地塞米松磷酸钠为内标.结果:头孢克洛在8～40μg·mL-1浓度范围内线性关系良好(r=0.999 8),平均回收率为 99.18% (n=5,RSD=1.69%).结论:本法简单、快捷、灵敏.     

高效毛细管电泳法测定一洗舒外用颗粒中咖啡酸的含量

建立以高效毛细管电泳法测定一洗舒外用颗粒中咖啡酸的含量.采用石英毛细管柱;运行缓冲液为20mmol·L-1的硼砂溶液(pH=9.18);分离电压12kV;真空进样时间为5s;温度为25℃,紫外检测波长313nm.结果显示,咖啡酸在20～100μg·mL-1范围内呈良好的线性关系,r= 0.9992;.咖啡酸的平均回收率均大于95%;RSD均小于3%(n=3).本方法操作简便、快捷、结果准确.     

HPLC测定小儿对乙酰氨基酚异丙嗪片的含量

目的 建立测定小儿对乙酰氨基酚异丙嗪片含量的高效液相色谱法.方法以Phenomenex Luna C18(4.6 mm×250mm,5μm)为色谱柱,甲醇-5 mmol·L-1己烷磺酸钠溶液一冰醋酸一三乙胺(6831.30.640.03)为流动相,流速为1.0mL·min-1,检测波长为306nm,进样量20μL.结果对乙酰氨基酚线性范围为0.929 7～4.648 mg·mL-1,r=0.999 9,平均回收率为99.96%(RSD=1.2%,n=9);盐酸异丙嗪线性范围为38.72～193.6 p.g·mL-1,r=0.999 9,平均回收率为99.38%(RSD=1.2%,n=9).结论 本法简便快速、准确可靠,可用于测定小儿对乙酰氨基酚异丙嗪片含量.     

HPLC法测定复方氨酚烷胺片中对乙酰氨基酚和咖啡因的含量

目的 采用HPLC法测定复方氨酚烷胺片中对乙酰氨基酚和咖啡因的含量.方法 采用十八烷基硅烷键和硅胶为固定相.以甲醇-0.05mml·L-1醋酸钠(38:62)为流动相;流速:1.0ml·min-1;检测波长为273nm.结果 对乙酰氨基酚和咖啡因的线性范围分别为25.0～250.0μg·mL-1(r=0.9999);1.5～15.0μg·mL-1(r=0.9999);对乙酰氨基酚的平均回收率为100.7%,RSD=0.9%;咖啡因的平均回收率为100.8%,RSD=1.5%.     

胶束毛细管电泳在线推扫法测定中成药中的士的宁

目的采用胶束毛细管电泳在线推扫法测定中成药中的微量士的宁。方法运行缓冲液为50 mmol.L-1NaH2PO4-90 mmol.L-1SDS-乙腈(83∶83∶34),pH2;0.5 psi压力进样,进样时间3.7 min;分离电压25 kV;分离温度25℃;检测波长205 nm。结果士的宁0.5～8.0μg.mL-1峰面积线性关系良好(r=0.9998),检测限达0.020μg.mL-1;方法回收率>97.6%;日内、日间RSD均小于1.8%。结论所用方法快速、准确,有效提高了毛细管电泳法的灵敏度。     

毛细管区带电泳法测定杜仲药材中绿原酸的含量

目的:建立采用高效毛细管电泳测定杜仲中有效成分绿原酸(CA)含量的方法,比较不同产地杜仲中绿原酸含量。方法:采用毛细管区带电泳(CZE),以内标法测定:运行电解质为含80mmol·L-1硼砂缓冲液-100mmol·L-1氢氧化钠(20∶1,pH=9.32),工作电压30kV,柱温25℃,检测波长为340nm,内标物为盐酸小檗碱。结果:绿原酸在0.006～0.574mg·mL-1的浓度范围内呈良好的线性关系(r=0.9994),平均回收率为101.43%,RSD为1.44%。结论:该方法简便、准确,重复性好。     

HPCE法测定归脾丸中远志皂苷元和远志酸的含量

目的:建立测定归脾丸中远志皂苷元和远志酸含量的高效毛细管电泳法。方法:采用未涂层毛细管柱(75μm×57 cm,有效长度50 cm),运行缓冲液为20 mmol.L-1硼砂溶液与20%甲醇(pH=8.0),分离电压25 kV,检测波长210 nm。结果:远志皂苷元、远志酸的线性范围分别为13.25～212μg.mL-1(r=0.9971)和12.5～200μg.mL-1(r=0.9977),平均回收率(n=5)分别为101.5%和100.4%。结论:本法简便、准确,重复性好,可用于归脾丸的质量控制。     

高效毛细管电泳法测定盐酸洛美沙星颗粒中洛美沙星的含量

目的:建立高效毛细管电泳法测定盐酸洛美沙星颗粒中洛美沙星的含量.方法:采用高效毛细管电泳法,电泳缓冲液为50 mmol·L-1硼砂-磷酸盐缓冲液(pH 8.5),检测波长为287 nm.结果:在20.0～120.0 mg·L-1间线性良好,相关系数r=0.999 8,日内和日间RSD分别为1.5%和2.6%,加样平均回收率为99.7%,洛美沙星的检测限为0.48 mg·L-1.结论:本方法能快速、简便、经济地测定盐酸洛美沙星颗粒中洛美沙星的含量,可用于临床检验和药物制剂的质量控制.     

毛细管区带电泳法测定岩陀中岩白菜素的含量

目的建立毛细管区带电泳法测定岩陀药材中岩白菜素的含量。方法岩陀药材用甲醇超声提取,采用未涂渍熔融石英毛细管(75μm×48.5 cm,有效长度40 cm),以25 mmol·L-1硼砂溶液为缓冲液,运行电压15 kV,温度25℃,内标为肉桂酸,检测波长为240 nm,运行时间10 min。结果岩白菜素与内标及其他成分能达到基线分离,在9.990⁴99.5μg·mL-1与峰面积呈良好的线性关系,Y=0.013 9X+0.005 6,r=0.999 6,检测限为4.995μg·mL-1(S/N=3),定量限为9.990μg·mL-1(S/N=10),平均加样回收率为101.1%(RSD=1.9%,n=6),低、中、高浓度日内、日间精密度RSD均<5%(n=3)。结论此方法可用于岩陀药材中岩白菜素的含量测定及质量控制,具有简便快速、准确可靠、试剂消耗量少的优点。     

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.