荧光法测定小鼠体内各组织中环丙沙星的浓度

目的:测定小鼠体内各组织中环丙沙星的浓度。方法:采用三氯化铝络合环丙沙星-荧光分光光度法。结果:在λ_(ex)=330 nm,λ_(em)=440 nm处,络合物的荧光值不受各组织的影响,且比环丙沙星自身的荧光值增加了20倍,线性范围为50～1000ng·mL~(-1)。结论:此方法准确、快速,适用于环丙沙星的体内研究。     

荧光猝灭法测定盐酸胺碘酮含量

目的:建立荧光猝灭法测定盐酸胺碘酮片剂含量的新方法。方法:试验多种荧光试剂加入系列浓度的胺碘酮溶液,测定其荧光光谱的变化。结果:选用芘丁酸(PBA)为荧光试剂,浓度为2.0mg·L~(-1),λ_(ex)/λ_(em)=349nm/376.3nm,在2.0～20mg·L~(-1)胺碘酮浓度范围与荧光猝灭值(F_0/F)成良好的线性关系(r=0.9962),据此提出测定片剂中胺碘酮含量的荧光猝灭法。结论:荧光猝灭法简便灵敏、选择性高,可用于药片中盐酸胺碘酮含量的测定。     

二阶导数光谱法测定鼻灵滴鼻剂中盐酸去氧肾上腺素的含量

目的建立鼻灵滴鼻剂中盐酸去氧肾上腺素的含量测定的二阶导数光谱法。方法采用二阶导数光谱法测定制剂中盐酸去氧肾上腺素的含量,λ=289nm,△λ=1nm,SLIT=2nm。结果在20~100mg·L~(-1)的范围内,振幅值(D)与浓度呈良好线性关系(r=0.9998)。回收率为100.2%,RSD为0.21%。结论本法可用于测定鼻灵滴鼻剂中盐酸去氧肾上腺素的含量。     

高效液相色谱-荧光检测法测定红景天苷的含量

目的:建立高效液相色谱-荧光检测法测定红景天苷的含量。方法:色谱柱为 Eclipse XDB-C_8柱(4.6 mm × 150 mm,5μm),流动相为水-甲醇(85:15),流速为1.0 mL·min~(-1),柱温为25℃,荧光检测波长λ_(EX)=220 nm,λ_(EM)=315 nm。结果:该方法的线性范围为1.00～500 ng(r=0.999 9)。平均加样回收率为 99.2％,RSD为 1.4％(n=5)。最低检测限为1.5 pg。结论:本方法快速,简单,灵敏度极高。     

荧光分光光度法测定何首乌及人参首乌胶囊中总蒽醌的含量

目的:建立测定何首乌及人参首乌胶囊中总蒽醌含量的方法。方法:荧光分光光度法。以最佳 pH 条件的无水乙醇为溶剂,在λ_(EX)=440nm、λ_(EM)=515nm 处测定总蒽醌含量。结果:在0.03～0.15μg·mL~(-1)范围内,大黄素浓度和荧光强度有良好的线性关系,回归方程为 F=194.36C 2.9642,r=0.9996。平均回收率何首乌为98.1%,RSD 为1.9%;人参首乌胶囊为98.6%,RSD 为2.0%。测得总蒽醌含量何首乌中为0.522 mg·g~(-1),人参首乌胶囊中为0.443mg·g~(-1)。结论:本法简便快捷,准确灵敏,重复性好,可用于何首乌及人参首乌胶囊的质量控制。     

离子对反相高效液相色谱法测定复合维生素粉中维生素B2和B6的含量

目的建立离子对反相高效液相色谱法,用于测定复合维生素粉中维生素B_2和B_6含量。方法用Dikma C_(18)柱(150 mm×4.6 mm,5μm),以甲醇:5 mmol·L~(-1)庚烷磺酸钠水溶液(含有0.5%冰醋酸和0.05%三乙胺)=30:70(V/V)为流动相,维生素B_2检测波长为265 nm,维生素B_6检测波长为λ_(ex)=295 nm,λ_(em)=397 nm,分离测定复合维生素粉中维生素B_2和B_6的含量。结果可直接测定出样品中维生素B_2和B_6的含量。维生素B_2的平均加样回收率为92.4%～98.4%,RSD为1.58%～3.12%(n=3),维生素B_6的平均加样回收率为96.0%～103.1%,RSD为1.21%～3.97%(n=3)。结论本方法准确、可靠,可用于复合维生素粉中维生素B_2和B_6含量的测定。     

离线紫外照射和高效液相色谱荧光法测定人血浆中他莫昔芬的浓度

目的建立测定人血浆中他莫昔芬的高效液相色谱荧光法。方法血浆样品经正己烷-正丁醇(98:2,V:V)提取后,以甲醇-1%三乙胺水溶液(82:18,V:V,pH 11.2)为流动相,流速为1 mL·min~(-1),色谱柱为Agilent Extend C_(18)(4.6 mm×150 mm,5μm),柱温为50℃,离线紫外照射(254 nm)10 min,荧光激发波长(λ_(ex))260 nm,发射波长(λ_(em))375 nm。结果血浆内源性杂质不干扰待测物测定,他莫昔芬的线性范围为0.5～200μg·L~(-1),定量下限为0.5μg·L~(-1),日内、日间精密度(RSD)均小于10%。样品反复冻融4次以及在提取后4℃下12 h内稳定性良好。结论该法灵敏、快速、准确、操作简便、线性范围宽,可用于他莫昔芬的药动学研究及临床治疗药物监测。     

高效毛细管电泳法测定清经胶囊中小檗碱含量

目的:采用高效毛细管电泳法(HPCE)的毛细管区带电泳分离模式(CZE)分离测定清经胶囊中小檗碱含量并与HPLC法比较。方法:熔融石英毛细管柱:58.5 cm(有效长度50 cm)×75μm;运行缓冲液:0.2 mol·L~(-1)乙酸钠溶液-甲醇(8:2);压力进样:20kPa·s;运行电压15 kV;柱上检测:λ=265 nm;毛细管柱温:25℃。结果:盐酸小檗碱进样浓度在9.95～159.2mg·L~(-1)范围内线性关系良好(r=0.999 9),平均加样回收率为100.4％(RSD=1.9％,n=5)。结论:该法与HPLC法所测结果吻合,但具有有机溶剂消耗少等优点,可用于清经胶囊中小檗碱含量的质量控制。     

甲癣搽剂中联苯苄唑和水杨酸的含量测定

目的:测定甲癣搽剂中联苯苄唑及水杨酸的含量。方法:采用双波长分光光度法测定其含量,测定波长在(254.0±0.5)nm,参比波长在(329.0±0.5)nm处测定联苯苄唑的含量;在波长(302.0±0.5)nm处测定水杨酸的含量。结果:联苯苄唑浓度在1.512～4.536 mg·L~(-1)范围内呈良好的线性关系。其回收率为99.5％,RSD为0.34％;水杨酸浓度在5.210～31.260 mg·L~(-1)范围内呈良好的线性关系。其回收率为98.5％,RSD为0.28％。结论:该实验方法简便,快速,操作简单,测定结果准确。     

胶束电动毛细管色谱法测定减肥保健品中的西布曲明、吲达帕胺、丁脲胺和氯噻嗪

目的:建立了胶束电动毛细管色谱法同时测定减肥保健品中的西布曲明、吲达帕胺、丁脲胺和氯噻嗪的方法。方法:以10.0 mmol·L~(-1)磷酸盐缓冲溶液-15.0 mmol·L~(-1)SDS(含35%乙腈,V/V,pH 7.5)为电泳介质,未涂层弹性石英毛细管(50μm×48cm,有效长度为40 cm)为分离通道,检测波长为210 nm,压力进样(5kPa×10s)。结果:西布曲明、吲达帕胺、丁脲胺和氯噻嗪的线性范围分别为4.0～100.0 m·L~(-1),2.0～80.0 mg·L~(-1),2.0～80.0 mg·L~(-1),2.0～80.0 mg·L~(-1),检出限分别为1.0,0.5,0.5,0.5 mg·L~(-1),5次重复测定的相对偏差为2.8%～4.5%;样品加标回收率为89%～103%。结论:该法简便快捷,准确可靠,用于中药成分减肥保健品分析,结果令人满意。     

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.