高效液相色谱法测定人血浆中利鲁唑的浓度

目的　建立测定人血浆中利鲁唑浓度的 HPL C法。 方法 　以美国迪马公司 Diamonsil〔 TM〕C1 8反相柱 ( 2 5 0 mm× 4.6mm,5μm)为色谱柱 ,流动相为甲醇 -0 .0 3 mol·L- 1磷酸二氢铵 ( 80∶ 2 0 ,V/V) ,流速为 0 .8m L·min- 1 ,检测波长 2 65 nm,以乙醚为提取剂。结果 　利鲁唑高 ( 80 0 ng·m L- 1 、中 ( 10 0 ng· m L- 1 )、低 ( 10 ng· m L- 1 ) 3个浓度的平均回收率分别为 98.3 6%、96.47%、95 .14 %,日内、日间差 RSD均低于 5 %( n=5 ) ;分析方法的定量测定下限为 5 ng·m L- 1。线性范围为 :5～ 10 0 0 ng·m L- 1 ,回归方程为 Y=2 14 .44 x-5 .89,r=0 .999( n=8)。结论 　该方法灵敏、准确、简单、快速 ,可用于临床血浓监测和药动学研究     

HPLC法测定恩普洛胶囊中丙磺舒的含量

目的　测定恩普洛胶囊中丙磺舒的含量。 方法 　高效液相色谱法 ;C8柱 (5μm.4.6× 15 0 mm) ;流动相为水 -乙腈 -1.0 mol· L- 1 磷酸二氢钾溶液 -1.0 mol· L- 1 醋酸溶液 (90 9∶ 690∶ 10∶ 1) ;流速 1.0 ml· min- 1 ;检测波长 2 5 4nm。结果 　丙磺舒在 2 5～ 2 0 0μg· ml- 1 范围内呈良好线性关系 (r=0 .99999) ,重现性良好 ,RSD=0 .1% (n=8) ,平均回收率 10 0 .0 % ,RSD=0 .5 % (n=9)。 结论 　本法操作简便 ,结果准确 ,重现性好     

高效液相色谱法测定利福喷丁胶囊的含量

目的　测定利福喷丁胶囊的含量。 方法 　高效液相色谱法 ,C8柱 (5 μm.4.6× 15 0 mm) ,流动相为甲醇 -乙腈 -0 .0 75 mol·L- 1磷酸二氢钾溶液 -1.0 mol·L- 1柠檬酸溶液 (2 80∶ 2 80∶ 2 60∶ 40 ) ,流速 1.0 ml· min- 1 ,检测波长 2 5 4nm。结果 　利福喷丁在 2 0～ 180 μg·ml- 1范围内呈良好线性关系 (r=0 .99999) ,重现性良好 RSD=0 .3 77% (n=10 ) ,平均回收率 99.7% ,RSD=0 .19(n=5 )。 结论 　本法操作简便 ,结果准确 ,重现性好。     

高效液相色谱法测定盐酸地匹福林眼用凝胶剂的含量

目的 :测定盐酸地匹福林 (DPE)眼用凝胶剂的含量。方法 :在ODS -C1 8色谱柱上采用流动相甲醇 - 0 0 2mol·L- 1 磷酸二氢钾溶液 (80∶2 0 ) ,波长 2 2 0nm进行检测。结果 :在 10 0～ 10 0 0 μg·mL- 1 范围内 ,DPE对照品的峰面积 (Y)与其浓度 (X)呈现良好的线性关系 ,r=0 9999,最低检测限 40ng·mL- 1 ,高、中、低 3种浓度平均回收率为 98 40 %～ 10 0 5 %(n =5 ) ,RSD分别为 1 17% ,1 15 % ,0 6 6 % ,平均日内、日间RSD分别为 0 70 % (n =6 )和 0 89% (n =5 )。结论 :本法快速、灵敏、准确、专属性高。     

RP-HPLC测定母体及胎儿血浆中罗哌卡因和布比卡因的药物浓度

目的 :建立罗哌卡因、布比卡因血浆药物浓度的反相高效液相 (RP HPLC)测定方法 ,并测定其母体和 (或 )胎儿血药浓度 ,为临床合理用药提供参考。方法 :采用AgilentHPLC系统 ;色谱柱 :Dikma C18(5 μm ,4 .6× 15 0mm)。以罗格列酮作为内标 ,流动相为磷酸二氢钠缓冲液 (10mmol·L- 1,pH3.0 )∶乙腈 =78∶2 2 ,流速 1.0mL·min- 1,λ =2 10nm。结果 :罗哌卡因线性关系为Y =0 .0 2 95X -0 .0 2 98(n =7,r =0 .9998) ;最低检测浓度为 0 .0 1mg·L- 1;平均回收率为 99.82 % ;日内、日间RSD分别小于 2 .4 7% ,3.75 % ;布比卡因线性关系为Y =0 .0 2 87X + 0 .0 2 71(n =7,r =0 .9998) ;最低检测浓度为 0 .0 1mg·L- 1;平均回收率为 10 1.0 1% ;日内、日间RSD分别小于 2 .6 9% ,4 .75 %。测定 6 0个血样 ,罗哌卡因浓度为 0 .15～ 0 .7mg·L- 1,布比卡因为 0 .1～ 0 .5 8mg·L- 1。结论 :RP HPLC法简便、灵敏、准确 ,可以用来测定临床血样中罗哌卡因、布比卡因的药物浓度 ,可为临床合理用药提供参考。     

高效液相色谱法测定人血浆中头孢羟氨苄浓度

用乙腈 -1mol·L- 1盐酸 ( 95∶ 5 )混合沉淀血浆蛋白 ,在 Spherisorb C18柱上 ,以 0 .0 15 mol·L- 1醋酸钠溶液 -甲醇 ( 94∶ 6 )为流动相进行分离 ,于 2 30 mm检测。结果表明 :线性范围为 1.0～ 6 4μg· m L- 1 ,加样回收率为 97.0 %～ 10 0 .2 % ,日内 RSD为 0 .89%～ 2 .2 4% ,日间 RSD为1.72 %～ 4.6 0 %。本法简便 ,准确 ,重现性好 ,可用于患者临床血药浓度检测     

HPLC法测定氯霉素滴眼液及其相关物质二醇物的含量

目的 　测定氯霉素滴眼液及其相关物质二醇物的含量。 方法 　采用高效液相色谱法。色谱柱 :Hypersil ODS( 15 0 mm× 4.6mm,5μm)( 0 .0 4mol· L- 1、p H7.0 )醋酸盐缓冲液 ;流速 :1.0 m L· min- 1 ;检测波长 :2 75 nm;进样量 10μL;柱温 40℃。 结果 　氯霉素在 2 0 .0～ 3 2 0 .0μg·m L- 1范围内线性关系良好 ( r=0 .9998) ,平均回收率为 10 0 .3 %;二醇物在 2 .0～ 3 2 .0 μg·m L- 1范围内线性关系良好 ( r=0 .9995 ) ,平均回收率为 99.7%;氯霉素 RSD( n=6)为 0 .9～ 1.6%,二醇物 RSD( n=6)为 1.1～ 1.7%。结论 　该法操作简便快速 ,结果准确性高 ,为药物生产、贮存过程中产品质量分析提供更简便快速的检测手段     

肠舒胶囊中阿魏酸含量的HPLC法测定

目的　建立肠舒胶囊中阿魏酸含量的HPL C测定方法。方法　选用 Hypersil C18分析柱(15 0 mm× 4 .6 mm,5μm) ,以甲醇为提取溶剂 ,甲醇- 10 m L· L-1冰醋酸 (2 3∶ 77)为流动相 ,检测波长32 0 nm,流速 1.0 m L· min-1。结果　线性范围 2 0～10 0 mg· L-1(r =0 .9999) ,平均回收率 97.5 % ,RSD 1.6 6 % (n =5 )。结论　本法测定肠舒胶囊中阿魏酸的含量 ,方法准确 ,简便 ,适用     

高效液相色谱法测定人血浆中头孢氨苄浓度

目的 　观察高效液相色谱法测定人血浆中头孢氨苄浓度的效果。 方法 　用乙腈 -1mol· L - 1盐酸 ( 95∶ 5 )混合沉淀血浆蛋白 ,在Spherisorb C1 8柱上 ,以水 -甲醇 -3 .86%醋酸钠溶液 -4 %酸醋溶液 ( 80 0∶ 2 0 0∶ 15∶ 3 )为流动相进行分离 ,于 2 5 4nm波长处检测。 结果 　线性范围为 1.0～ 12 8.0 μg·m L- 1 ,加样回收率为 97.5 %～ 10 0 .5 %,日内 RSD为 0 .98%～ 1.82 %,日间 RSD为 1.85 %～ 4.93 %。结论 　本法简便 ,准确 ,重现性好 ,可用于患者临床血药浓度检测     

高效液相色谱法分析阿奇霉素的含量

目的 　建立 HPLC方法测定阿奇霉素的含量。方法 　采用 Agilent Hypersil ODS C1 8色谱柱 ( 4 .0 mm× 2 5 0 mm,5 μm) ,0 .1mol· L- 1磷酸二氢铵溶液 (三乙胺调节 p H值为 6.5 ) -乙腈 ( 70∶ 3 0 )为流动相 ,流速 1.0 m L·m in- 1 ,检测波长为 2 12 nm。 结果 　阿奇霉素的浓度在 0 .4～4.0 mg· m L- 1范围内线性关系良好 ,回归方程为 :Y=171.0 1X-12 .5 2 3 ,r=0 .9998( n=6) ;平均回收率为 99.6% ,RSD为 1.2 2 % ( n=6)。结论　本方法简单、快速、准确。     

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.

     

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.     

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.     

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.