反相高效液相色谱法测定复方谷氨酰胺中呱仑酸钠的含量

目的 :建立复方谷氨酰胺中呱仑酸钠的反相高效液相色谱测定方法。方法 :色谱柱InertsilCN 3(5μm ,4.6mm× 2 50mm) ,磷酸盐缓冲液 (pH 7) 乙腈 (50∶50 )为流动相 ,检测波长 2 90nm ,流速1 .0mL·min- 1 。结果 :呱仑酸钠的浓度在 1 .0～ 6 .0mg·L- 1 范围内呈线形关系 ,平均回收率为 99.8% ,RSD为 0 .4 % (n =8)。结论 :本法具方法简便 ,结果准确 ,适用于制剂中呱仑酸钠的含量测定和质量控制     

呱仑酸钠血药浓度HPLC测定方法研究

目的 :建立水溶性药物呱仑酸钠血药浓度的高效液相色谱分析方法。方法 :以对二甲氨基苯甲醛为内标 ,在比较了固相萃取、离子对萃取及沉淀蛋白 -脱水法等 3种预处理方法的基础上 ,采用沉淀蛋白 -脱水法预处理兔血浆样品 ,分析柱为 μBondapakC18柱 (2 5 0mm× 4 6mm ,10 μm) ,流动相为 pH 7 0的 0 0 1mol·L-1磷酸盐缓冲液 -甲醇 (5 0∶5 0 ) ,流速1mL·min-1,在 2 93nm波长处检测 ,按内标法定量。结果 :血药浓度线性范围为 0 1～ 10 0mg·L-1(r=0 9997) ,最低检测浓度为 0 0 2mg·L-1(S/N >3) ,萃取回收率在 79 5 %～ 86 4% (n =5 ) ,分析方法回收率在 93 1%～ 95 5 % (n =5 ) ,日内和日间RSD分别为 1 2 %～ 1 8%和 1 9%～ 3 1% (n =5 )。结论 :本法简便、准确、精密度高、重现性好 ,适用于呱仑酸钠的体内研究     

高效液相色谱法测定卡马西平片的含量

建立卡马西平片含量测定的HPLC方法。色谱柱为LichrosorbDiol (4 0× 2 5 0mm ,5 μm ) ;流动相 :乙腈 -甲醇 - 0 0 5 %冰醋酸溶液 (5∶5∶90 ) ;流速 :1 0ml·min-1;检测波长 :2 30nm ;柱温 :2 5℃ ;峰面积外标法。卡马西平在 10～ 10 0 μg·ml-1范围内具有良好的线性关系 ,回归方程为A =1 6 95 3× 10 4C - 2 5 5 5 5× 10 3 ,r=0 99997;平均回收率为 99 6 9% ,RSD =0 75 % (n =6 )。本法准确可靠 ,专属性强 ,能更好地控制其质量。     

HPLC法测定茵栀黄软胶囊中黄芩苷、栀子苷和绿原酸的含量

目的测定茵栀黄软胶囊中的 3种有效成分 ,黄芩苷、栀子苷、绿原酸的含量。方法HPLC法 ,Irregular HC18(2 5 0 . 0mm× 4 6mm ,10 μm)色谱柱。黄芩苷流动相 :甲醇 水 磷酸 (V∶V∶V =4 7. 0∶5 .3 0∶0. 2 ) ,流速 :1 0mL·min-1,检测波长 :2 80nm ;栀子苷流动相 :乙睛 水 (V∶V =15∶85 ) ,流速 :1 0mL·min-1,检测波长 :2 38nm ;绿原酸流动相 :乙睛 磷酸溶液 (w =0 . 4 % )(V∶V =13∶87) ,流速 :1 0mL·min-1,检测波长 :32 7nm。结果黄芩苷在 2 7 5～ 137 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =6 4. 83× 10 4ρ - 1 6. 96× 10 .5 ,r =0 . 9998,平均回收率为 99 4 6 % (RSD =1 0 1% ) ;栀子苷在 16 .5～ 82 . 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =8 794× 10 .5ρ - 4 . 116× 10 2 ,r =0 . 9999,平均回收率为 10 0 . 37% (RSD =1 4 .0 % ) ;绿原酸在 2 4～ 12 0mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =2 4 88× 10 4ρ - 9 2 4 4× 10 4,r =0 9999,平均回收率为 99 38%(RSD =1. 89% )。结论测定方法可用于茵栀黄软胶囊的质量控制。     

混合滥用药物的气相色谱质谱分析

目的 :建立混合滥用药物快速、灵敏检测方法。方法 :采用气相色谱 质谱法 (GC MS)对 11种毒品、药品进行定性定量分析。结果 :苯丙胺类及吗啡在 5 0× 10 - 4- 2 0× 10 - 2 g·ml- 1 范围内线性关系良好 ,检出限分别为 1 0×10 - 4g·ml- 1 和 2 0× 10 - 4g·ml- 1 ;氯胺酮、哌替啶、地西泮、咖啡因、可卡因、马来酸氯苯吡及乙酰替乙氧苯胺线性范围为 5 0× 10 - 6 - 5 0× 10 - 4g·ml- 1 ,检出限为 1 0× 10 - 6 g·ml- 1 和 2 0× 10 - 6 g·ml- 1 。结论 :本方法可用于混合滥用药物组分的快速、准确定性定量分析。     

HPLC测定盐酸小檗碱片的含量

目的　建立盐酸小檗碱片的含量测定方法。方法　采用HPLC法 ,选用InertsilODS - 3C18色谱柱 (2 5 0mm× 4 .6mm ,5μm) ,0 .0 33mol·L-1KH2 PO4溶液 -乙腈 (6 5∶35 )为流动相 ,检测波长为 2 6 5nm。结果　盐酸小檗碱在 0 .2～ 1.6 μg·ml-1浓度范围内线性关系良好。回归方程为 :A =4 .2 12× 10 6C - 1.0 0 9× 10 5(r=0 .9999)。结论　所用方法简便、快速 ,结果准确。     

HPLC法测定苯噻啶含量及其有关物质

本文采用HPLC法测定苯噻啶对照品含量及其有关物质。色谱柱KromasilC18(2 5 0× 4 6mm ,5 μm) ,流动相 :乙腈 -水 -三乙胺 (5 5∶4 5∶0 2 ,磷酸调节溶液pH3 5 ) ,检测波长 :2 5 4nm ,流速 :1 0ml·min-1,进样量 :2 0 μl。苯噻啶在浓度 6 5～ 2 0 8μg·ml-1浓度范围内线性关系良好。回归方程A =64185 74 +81992 3C ,r=0 99998。平均回收率 10 0 1% (n =6) ,RSD为 0 5 8%。本法简便、灵敏、准确     

RP-HPLC测定替拉扎明及其有关物质

目的　建立测定替拉扎明含量及其有关物质检查的高效液相色谱法。方法　采用HypersilC18色谱柱(2 5 0mm× 4.6mm ,id 10 μm) ,甲醇 - 5 0mmol·L-1磷酸盐缓冲液 (10∶90 ,氢氧化钠调pH =6 .5± 0 .1)为流动相 ,在检测波长 2 6 6nm处进行含量测定 ;在相同条件下 ,以甲醇 - 5 0mmol·L-1磷酸盐缓冲液 (2 5∶75 ,氢氧化钠调pH =6 .5±0 .1)为流动相 ,对有关物质进行检查。结果　替拉扎明在 1.2 7～ 5 0 .8μg·ml-1范围内 ,峰面积与其浓度线性关系良好 (r =0 .9999) ,最低检测限为 2 .5× 10 -2 ng (S/N =3) ,重复进样RSD =0 .6 9% (n =5 ) ,日内RSD =0 .83%(n =5 ) ,日间RSD =0 .39% (n =5 ) ,重复性试验RSD =0 .2 1% (n =6 ) ,加样回收率为 99.6 2 %。结论　本法准确、简便、快速 ,可用于替拉扎明原料药及其制剂的质量控制     

HPLC测定盐酸土霉素的含量和有关物质

目的 :建立HPLC测定盐酸土霉素有关物质和含量。方法 :采用ODS柱 ( 10 μm ,4 6mm× 2 5 0mm) ,以 0 1mo1·L-1草酸铵溶液 二甲基甲酰胺 0 2mo1·L-1磷酸氢二铵溶液 ( 6 0∶30∶10 ) (用氨试液调pH8 3)为流动相 ,检测波长 2 70nm。结果 :盐酸土霉素在 0 1～ 1 0mg·ml-1浓度范围内 ,呈良好的线性关系 (r =0 9999) ,精密度RSD为1 2 % ,平均回收率为 99 6 % ,RSD为 0 8% (n =4)。结论 :该法简便、准确 ,适用于盐酸土霉素杂质的检测和含量的测定。     

高效液相色谱法测定奥卡西平及片剂的含量和有关物质

目的 :用高效液相色谱法测定奥卡西平及片剂的含量和有关物质。方法 :采用DiamonsilC18(2 0 0mm× 4.6mm ,5 μm)色谱柱 ,流动相 :乙腈 0 .0 5mol·L 1磷酸二氢钾 (磷酸调 pH为 3.0 ) (4 0 :6 0 ) ,检测波长 :2 5 6nm ,柱温 :40℃ ,流速 :1.0ml.min 1,峰面积外标法。结果 :在 12 .5～ 112 .5 μg .ml 1的奥卡西平浓度范围内 ,峰面积与浓度呈良好的线性关系 ,回归方程 :Y =3.2×10 5C - 2 .6 1× 10 3 相关系数r=0 .9996 ;片剂中奥卡西平平均回收率为 99.7% (n =5 ) ,RSD =0 .33%。结论 :方法简便 ,快速 ,准确。可同时分离和测定奥卡西平原料及其片剂中各杂质及主药含量     

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.     

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.     

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.