高效液相色谱法测定强力救心滴丸中丹参素钠的含量

目的:测定强力救心滴丸中丹参素钠的含量。方法:采用高效液相色谱法。色谱柱为Kromasil C_(18)柱(250mm×4.6mm5μm);水-甲醇-二甲基甲酰胺-冰醋酸(95:5:2:1)为流动相,流速:1.0ml·min~(-1);检测波长280nm;柱温:25℃。结果:丹参素钠在0.25～2.200μg范围内具有良好线性关系。平均回收率为97.46％,RSD为3.01％。结论:该法可用于强力救心滴丸中丹参素钠的含量测定。     

离子对—HPLC法测定盐酸二甲双胍含量及有关物质

目的:建立离子对-HPLC法测定盐酸二甲双胍含量及有关物质的方法。方法:采用Inertsil C_(18)色谱柱(5μm,4.6mm×150mm);以甲醇-5mmol·L~(-1)磷酸二氢钾溶液(含有10mmol·L~(-1)十二烷基磺酸钠,用磷酸调节pH至3.5±0.05),(64:36)为流动相;流速1.0mL·min~(-1);紫外检测波长:233nm用于含量测定,218nm用于有关物质检测;柱温:室温。结果:离子对-HPLC法测定盐酸二甲双胍的线性范围为5～500μg·mL~(-1);相关系数r=0.999 9;日内精密度RSD=0.82％,日间精密度RSD=1.9％(n=5);双氰胺的线性范围为0.08～0.80μg·mL~(-1);相关系数r=0.9999;日内精密度RSD=0.68％,日间精密度RSD=2.3％(n=5);盐酸二甲双胍含量测定高、中、低3种浓度的回收率分别为99.24％,99.53％,99.18％;RSD分别为0.15％,0.18％,0.22％。结论:本法简便、快速、准确、专属性好。     

高效液相色谱法测定替硝唑凝胶剂的含量

目的:制备替硝唑外用凝胶;并以甲硝唑为内标,采用高效液相色谱法测定替硝唑凝胶剂的含量。方法:采用Hyper-sil-C_(18)柱(5μm,5mm×250mm);以甲醇-水-36％醋酸(30:70:0.5)为流动相;流速为1.0mL·min~(-1);检测波长为318nm;灵敏度为0.08 AUFS。结果:替硝唑浓度在41.84～125.52mg·L~(-1)范围内呈良好的线性关系,r=0.9997;平均回收率为97.92％,RSD为1.02％。结论:该方法快速,准确,重现性好,适用于替硝唑凝胶剂的质量控制。     

RP-HPLC法测定氢溴酸加兰他敏口服液含量及有关物质

目的:采用反相高效液相色谱法测定氢溴酸加兰他敏的含量及其有关物质。方法:采用Kromasil C_(18)色谱柱(5 μm,4.6mm×150 mm);以乙腈-水相(20:80,每 800 mL水相中含有2.67 mL 二丁胺,用磷酸调节pH为 9.0±0.05)为流动相;流速1.0 mL·min~(-1);检测波长:280 nm;柱温:室温;进样量:20 μL。结果:反相高效液相色谱法测定的线性范围为30～210 μg·mL~(-1);r=0.999 9;日内精密度:RSD为0.73％(n=5);日间精密度:RSD为0.72％(n=5),氢溴酸加兰他敏含量测定高、中、低3种浓度的回收率分别为98.89％、99、84％和99.56％,RSD分别为0.53％、0.40％和0.49％。结论:本法简便快速、准确、专属性好。     

RP-HPLC法测定注射用甲砜霉素甘氨酸酯盐酸盐的含量和有关物质

目的:采用反相高效液相色谱法测定注射用甲砜霉素甘氨酸酯盐酸盐(TGH)含量及有关物质。方法:采用色谱柱:Diamonsil C18柱(250 mm×4．6 mm,5μm);流动相:0．01 mol·L-1三氟乙酸-乙腈(88:12);流速: 1．0 mL·min-1;紫外检测波长:223 nm;进样体积:20μL;柱温:40℃。结果:含量测定的线性范围为40—400μg·mL-1,r=0．999 9(n=5),注射用TGH的加样回收率为98．4％-100．3％;RSD在0．29％-1．08％。结论:本法简便快速、准确,专属性好。     

反相高效液相法测定苦参素脂质体药物含量及包封率

目的:建立苦参素脂质体中药物含量及包封率测定的反相高效液相(RP-HPLC)法。方法:采用Di-monsil~(TM)ODS柱(200mm×4.6mm,5μm);流动相为乙腈-0.1％N_3PO_4水溶液(用三乙胺调pH3.13)(5:95);柱温:室温;流速:1mL·min~(-1);紫外检测波长:215nm。采用Sephadex G-50分离苦参素脂质体中的游离药物。结果:在本色谱条件下苦参素与辅料及溶剂峰分离良好,苦参素在20～100μg·mL~(-1)范围内线性关系良好(r=0.9999,n=5),回收率在99.90％～102.0％之间,日内RSD及日间RSD均小于2％(n=5)。结论:该方法准确可靠、简单快速,可用于苦参素脂质体含量及包封率的测定。     

HPLC法测定鄂天麻2号中天麻素含量

目的:建立鄂天麻2号中天麻素的含量测定方法。方法:采用高效液相色谱法,色谱柱为Diamonsil C_(18)柱(250 mm×4．6 mm,5μm);流动相为甲醇-磷酸盐溶液(0．1 mol·L~(-1)磷酸氢二钠和0．1 mol·L~(-1)磷酸二氢钾溶液等量混合)-水(1．5:3: 95．5);检测波长270 nm;柱温为室温;进样量10μl。结果:天麻素线性范围:0．152-5．003μg,r=O．999 9。鄂天麻2号中天麻素的含量为0．84％。结论:该方法分离度好,快速简便,鄂天麻2号药用质量较高。     

HPLC法测定萘哌地尔片的含量

目的:建立萘哌地尔片含量测定的HPLC法。方法:采用Hypersil C_(18)色谱柱(4.6 mm×200 mm,5 μm),以乙腈-甲醇-0.02mol·L~(-1)醋酸钠缓冲液(45:5:22)为流动相,流速为1.0mL·min~(-1),检测波长为232nm,柱温为室温,进样体积为20μL。结果:线性范围为2.0～20.0μg·mL~(-1)(r=0.9999,n=5);高、中。低3种不同浓度的平均回收率范围为100.2％～100.4％,RSD为0.26％～0.46％;精密度为0.32％(n=5)。结论:本法快速、准确、专属性高,适于萘哌地尔片的含量测定。     

HPLC法测定氟尿嘧啶-羟丙基-β-环糊精包合物温敏凝胶剂的含量

目的:制备氟尿嘧啶(5-Fu)-羟丙基-β-环糊精包合物阴道用温敏凝胶剂,并采用高效液相色谱法测定5-Fu的含量.方法:采用Hypersil-C18柱((150 mm×4.6 mm,5μm);以水(用0.05 mol· L-1磷酸溶液调节pH至3.5)-甲醇(95:5)为流动相;流速为1.0 ml·min-1;检测波长:266 nm;柱温25℃;进样量为20μl.结果:5-Fu在0.6～ 18 μg· ml-1浓度范围内线性关系良好(r=0.999 8),平均回收率为100.45％,RSD为1.05％(n=9).3批样品中5-Fu的平均含量为102.70％.结论:本检测方法灵敏、快速、结果准确,适用于5-Fu凝胶剂的质量控制.     

固相萃取—HPLC法测定法莫替丁血药浓度

目的:建立法莫替丁血药浓度测定方法。方法:采用固相萃取高效液相色谱法。样品先经Waters Oasis HLB固相萃取小柱处理。色谱柱:Shim-pack C_8 150mm×4.6mm,10μm;柱温:35℃;流动相为乙腈-0.019mol·L~(-1)磷酸(10:90);流速:1mL·min~(-1);检测波长:265nm。结果:线性范围5～200μg·L~(-1),线性关系良好,最小可测定浓度为5μg·L~(-1)。回收率80％以上,日内及日间RSD小于10％。结论:采用新型固相萃取柱能快速可靠地测定法莫替丁血药浓度。     

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.