RP-HPLC法同时测定壳聚糖止血海绵中3组分的含量

目的:建立壳聚糖止血海绵中地塞米松磷酸钠、替硝唑及克林霉素的RP-HPLC含量测定方法。方法:色谱柱为Dis- covery C18柱(150 mm×4．6 mm,5μm);流动相为乙腈-0．05 mol·L-1磷酸二氢钾缓冲液-三乙胺(35:65:0．3),用磷酸调pH至5．3;流速1．0 ml·min-1;检测波长210 nm。结果:地塞米松磷酸钠、替硝唑、克林霉素分别在2-10μg·ml-1(r=0．999 7)、6 -30μg·ml-1(r=0．999 8)、30-150μg·ml-1(r=0．999 8)线性范围内呈现良好的线性关系。3组分的平均回收率分别为99．4％(RSD=2．1％);98．7％(RSD=1．7％)、99．2％(RSD=1．9％)。结论:本法操作简便、快速、结果准确。可作为该制剂的质控方法。     

HPLC法测定复方硫酸新霉素滴眼液中地塞米松磷酸钠的含量

目的:建立HPLC法测定复方硫酸新霉素滴眼液中地塞米松磷酸钠的含量。方法:采用Eclipse XDB-C18色谱柱(250 mm×4．6mm,5μm),流动相为0．75％三乙胺溶液-甲醇-乙腈(40:55:5)流速1．0 ml·min-1,检测波长为242 nm。结果:地塞米松磷酸钠在0．1～1．21μg的范围内线性关系良好(r=0．999 8),平均回收率为99．0％,RSD为1．6％。结论:该法简便、快捷、准确,能更好的控制其质量。     

HPLC法测定氨酚比林注射液中对乙酰氨基酚和氨基比林的含量

目的:建立氨酚比林注射液中对乙酰氨基酚、氨基比林含量的高效液相色谱方法。方法:选用AgilentSBC18(150 mm ×4．6mm,5μm),乙腈-0．1％磷酸溶液-三乙胺(12:87:1)为流动相,检测波长为240 nm,流速为1．0 ml·min-1。结果:对乙酰氨基酚的线性范围为0．35-1．74μg(r=0．999 9),平均回收率为101．4％,RSD=0．5％;氨基比林的线性范围为0．48～2．42 μg,r=0．999 9,平均回收率为100．3％,RSD=0．4％。结论:本方法快速、准确,样品处理简便易行。     

高效液相色谱法测定萝藤安神片中钩藤碱的含量

目的:建立藤安神片中钩藤碱的HPLC测定方法。方法:Diamonsil ODS C18(200mm×4．6 mm,5μm)柱,甲醇-水(48:52)含10 mmol·L-1三乙胺溶液,用醋酸调pH=5．0为流动相,流速1．0 ml·min-1检测波长为254 nm。结果:钧藤碱的线性范围是0．20-0．99μg(r=0．999 8),平均回收率为97．9％,RSD=1．0％。结论:方法简单准确,可作为该制剂的质量控制。     

RP-HPLC法测定匹林咖敏片中马来酸氯苯那敏的含量

目的:建立匹林咖敏片中马来酸氯苯那敏的RP-HPLC测定方法。方法:用Kromasil C18色谱柱(250 mm×4．6 mm,5μm),以乙腈-0．3％十二烷基硫酸钠溶液-磷酸(60:40:0．02)(用三乙胺调pH至3．5)为流动相,流速为1．0 ml·min-1,检测波长为264 nm。结果:马来酸氯苯那敏在20．21-60．63μg·ml-1范围内呈线性关系,r=0．999 9,平均回收率为99．7％,RSD= 0．4％(n=9)。结论:本法适用于匹林咖敏片中马来酸氯苯那敏的含量测定。     

HPLC法测定消喘膏中延胡索乙素的含量

目的:测定消喘膏中延胡索乙素的含量。方法:色谱柱为Dikma Diamonsil C18(200mm×4．6mm,5μm),流动相为甲醇-0．1％磷酸溶液(三乙胺调pH值至6．0)(55:45),流速为1．0ml·min-1,检测波长为280nm。结果:延胡索乙素进样量在0．051μg-1．020μg范围内与峰面积呈良好的线性关系(r=0．9999),平均回收率为99．35％(n=9)．RSD为0．75%。结论:本方法简便快速,分离度好,结果准确可靠。     

HPLC法测定五维赖氨酸颗粒中四种维生素的含量

目的:建立离子对RP-HPLC法测定五维赖氨酸颗粒中烟酰胺、维生素B6、维生素B2、维生素B1的含量。方法:用Zorbax Eclipe XDB-C18柱(250 mm×4．6 mm,5μm),流动相为0．005 mol·L-1庚烷磺酸钠溶液(含0．5％冰醋酸和0．05％三乙胺)-甲醇(72:28)为流动相,流速为1．0 ml·min-1,检测波长为280 nm。结果:烟酰胺、维生素B6、维生素B2及维生素B1的线性范围分别为0．32-15．77μg(r=0．999 7),0．05～2．61μg(r=0．999 9)、0．05-2．65μg(r=0．999 9)及0．45-22．37μg(r= 0．999 9),平均回收率分别为98．3％(RSD 1．3％,n=9)、101．1％(RSD 1．9％,n=9)、99．3％(RSD 1．0％,n=9)、98．9％(RSD 1．1％,n=9)。结论:本法简便,快速,可用于五维赖氨酸颗粒产品的质量控制。     

高效液相色谱法测定那氟沙星乳膏含量

目的:采用高效液相色谱法测定那氟沙星乳膏的含量。方法:Diamonsil C18柱(250 mm×4．6 mm,5μm)为分析柱;乙腈-四氢呋喃-0．025 mol·L-1磷酸二氢铵溶液(35:5:60),用磷酸调节pH至3．0为流动相;流速1．0 ml·min-1,检测波长280 nm。结果:那氟沙星在2．5-25μg·ml-1范围内呈良好线性关系,r=0．999 9,平均回收率=99．2％,RSD=0．7％(n=9)。结论:本方法简单、快捷、结果可靠。     

反相高效液相色谱法测定头孢克肟口含片中头孢克肟的含量

目的:建立RP-HPLC测定头孢克肟口含片中头孢克肟含量的方法。方法:色谱柱为ReliaSil C_18(250 mm×4．6 mm, 5μm),流动相为四丁基氢氧化铵溶液(用1．5 mol·L~(-1)磷酸溶液调节pH至7．0)-乙腈(70:30),检测波长254nm。流速0．8 ml·min~(-1)。结果:头孢克肟浓度在2-120μg·ml~(-1)范围内,与峰面积呈良好的线性关系,r=0．999 9;平均回收率为100．6％(n= 9),RSD=1．4％。结论:该方法简便可靠,可用于头孢克肟口含片的质量控制。     

高效液相色谱法测定消石利胆浓缩丸中芍药苷的含量

目的:建立HPLC法测定消石利胆浓缩丸中芍药苷的含量。方法:使用Lichrosorb C18色谱柱(250 mm×4．6 mm,5μm),以甲醇-0．05 mol·L-1磷酸二氢钾溶液-三乙胺(28∶72∶0．5)为流动相,流速为1．0 ml·min-1,检测波长为230 nm。结果:芍药苷在0．39～0．92μg范围内呈线性关系,r=0．999 9,平均回收率为98．4％,RSD为2．0％。结论:该方法简便,重复性好,可用于该药的质量控制。     

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.     

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.