RP-HPLC测定氨苄西林丙磺舒胶囊中的有关物质

目的 建立氨苄西林丙磺舒胶囊有关物质的RP-HPLC梯度洗脱方法.方法 色谱柱为十八烷基硅烷键合硅胶柱;流动相A为2 mol/L醋酸溶液-0.2 mol/L磷酸二氢钾溶液-乙腈-水(0.5:50:50:900);流动相B为2 mol/L醋酸溶液-0.2 mol/L磷酸二氢钾溶液-乙腈-水(0.5:50:400:550),流速为1 ml/min,线性梯度洗脱;检测波长为254 nm,柱温40℃,进样器15℃,进样量为20 μl.结果 该方法能专属、准确地测定氨苄西林丙磺舒胶囊中的有关物质.结论 本色谱条件适合氨苄西林丙磺舒胶囊有关物质的测定,可纳入氨苄西林丙磺舒胶囊质量标准.     

HPLC法测定氨苄西林丙磺舒胶囊有关物质

目的建立氨苄西林丙磺舒胶囊有关物质的HPLC测定方法。方法采用Waters-C18柱(150mm×4.6mm,5μm,W03061M029),流动相A为12%醋酸溶液-0.2mol.L-1磷酸二氢钾溶液-乙腈-水(0.5∶50∶50∶900),流动相B为12%醋酸溶液-0.2mol.L-1磷酸二氢钾溶液-乙腈-水(0.5∶50∶400∶550),流速:1.0mL.min-1;检测波长为230nm。结果在选定条件下,有关物质与氨苄西林、丙磺舒二主药完全分离,氨苄西林在0.1~1.6mg.mL-1、丙磺舒在0.028~0.448mg.mL-1范围内线性关系良好。结论本法简便、准确,重现性好,可用于氨苄西林丙磺舒胶囊有关物质的检测。     

反相高效液相色谱法分析注射用氨苄西林钠有关物质

目的采用反相高效液相色谱法测定注射用氨苄西林钠有关物质,并对有关物质进行分析。方法采用Ultimate TM XB C18（5μm,4.6mm×250mm）色谱柱,流动相A为12%醋酸溶液-0.2mol/L磷酸二氢钾溶液-乙腈-水（0.5：50：50：900）;流动相B为12%醋酸溶液-0.2mol/L磷酸二氢钾溶液-乙腈-水（0.5：50：400：550）;柱温：35℃;流速：1.0ml/min;检测波长：254nm。结果氨苄西林与有关物质可完全分离,L-氨苄西林、氨苄西林开环二聚物、氨苄西林闭环二聚物分别在相对主峰保留时间为0.7、2.8、3.5倍处出峰。结论定位注射用氨苄西林钠三种杂质峰位。     

反相高效液相色谱梯度洗脱法测定注射用氨苄西林钠舒巴坦钠有关物质

目的 建立用反相高效液相色谱梯度洗脱法测定注射用氨苄西林钠舒巴坦钠有关物质.方法 色谱柱为十八烷基硅烷键合硅胶柱(UltimateTM AQ-C18,4.6mm×250mm,5μm),检测波长为254nm,采用A相[12%乙酸溶液:0.2mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:50:900)]-B相[(12%乙酸溶液:0.2mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:400:550)]为流动相进行梯度洗脱(A相起始比例为90%,保持15min,25min内下降至0,保持该比例10min),流速为1.0ml/min,柱温为25℃,进样量为20μl.结果 舒巴坦的碱性降解产物(舒巴坦青霉胺)、舒巴坦、氨苄西林的碱性降解产物、氨苄西林、头孢拉定和氨苄西林二聚物等相关物质在本色谱条件下均能实现较好分离,杂质相对检出率较高.结论 本法基线稳定,重现性好,准确度高,可同时测定氨苄西林钠舒巴坦钠的有关物质.     

高效液相梯度洗脱法测定氨苄西林丙磺舒分散片中的有关物质

目的:用高效液相色谱法测定氨苄西林丙磺舒分散片中的有关物质.方法:色谱柱为十八烷基硅烷键合硅胶柱;检测波长232 nm;采用A相(含20%磷酸盐缓冲液的乙腈溶液)-B相磷酸盐缓冲液[水-1 mol·L-1磷酸二氢钾溶液-1 mol·L-1醋酸溶液(909:10:1)]为流动相进行梯度洗脱(A相的起始比例为10%,30 min内上升至90%);流速为1 mL·min-1;柱温为30℃;进样量为10μL.结果:本法实现了在较短时间内将原料中引入的有关物质和强力破坏条件下产生的降解产物与主成分之间的基线分离.结论:本色谱条件适合氨苄西林丙磺舒分散片中的有关物质的测定.     

HPLC法测定注射用氨苄西林钠舒巴坦钠中聚合物

目的建立反相高效液相色谱梯度洗脱法,测定注射用氨苄西林钠舒巴坦钠中的二聚物。方法采用Diamonsil C18(250 mm×4.6 mm,5μm)。流动相:A相[12%醋酸溶液:0.2 mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:50:900)];B相[12%醋酸溶液:0.2 mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:400:550)]。梯度洗脱(A相起始比例为85%,保持8.5 min,30 min内下降至0,保持该比例15 min),流速为1.0 mL/min,检测波长为254 nm。结果氨苄西林在0.675～5.4 mg/mL范围内与氨苄西林二聚物峰面积呈良好的线性关系(r=1.0000)。结论该方法能较好地分离舒巴坦、氨苄西林、氨苄西林二聚物及其他杂质,方法简便,结果可靠,可用于注射用氨苄西林钠舒巴坦钠中氨苄西林二聚物的检测。     

HPLC法测定一次性输液器中可沥滤物苯酞和苯酚

建立了HPLC法检测一次性输液器中的可沥滤物苯酞和苯酚.采用YMC-PackPro C18色谱柱,流动相A为0.04 mol/L的磷酸二氢钾和0.2％三乙胺溶液:乙腈:异丙醇(92:4:4),流动相B为0.04 mol/L的磷酸二氢钾和0.2％三乙胺溶液(pH 6.6):乙腈(40:60),梯度洗脱,检测波长为220 ...     

高效液相色谱法测定氨苄西林/丙磺舒胶囊中氨苄西林、丙磺舒的含量

目的:建立测定氨苄西林/丙磺舒胶囊中氨苄西林、丙磺舒含量的高效液相色谱法(HPLC法)。方法:采用Waters2690-2487型高效液相色谱仪,SymmetryShieldTMRP18柱(150mm×3.9mm,5μm)。氨苄西林流动相为0.068mol/L的磷酸二氢钾溶液(pH=3.0)-乙腈(92∶8,V/V);丙磺舒流动相为水-乙腈-1mol/L磷酸二氢钾溶液-1mol/L冰醋酸(59.5∶39.8∶0.62∶0.08,V/V),加入0.15%的三乙胺调节pH=2.76;流速均为1.4mL/min。氨苄西林检测波长为210nm,丙磺舒检测波长为254nm。结果:氨苄西林的浓度线性范围为1.25～40μg/mL(r=0.9999),丙磺舒的浓度线性范围为0.308～10μg/mL(r=0.9999)。结论:HPLC法操作简便、灵敏、快速、重现性好,适用于该产品中氨苄西林、丙磺舒含量的测定。     

HPLC-UV法测定丁苯那嗪原料药中的有关物质

首次建立高效液相色谱-紫外检测(HPLC-UV)双波长法测定丁苯那嗪原料药中7 个有关物质.采用Welch Ultimate XB-C18 色谱柱,以0.005 mol/L 磷酸氢二钾和0.005 mol/L 磷酸二氢钾溶液(pH 7.0)为流动相A,乙腈为流动相B,梯度洗脱,检测波长为284nm、220 nm.结果表...     

氨苄西林丙磺舒胶囊的HPLC测定

建立了HPLC法测定氨苄西林丙磺舒胶囊的含量.采用C18色谱柱,以甲醇-0.02mol/L磷酸二氢钾溶液(用磷酸调至pH 3.0)(50:50)为流动相,检测波长232nm,流速lml/min.氨苄西林和丙磺舒分别在80～800μg/ml(r=0.9992)和22～220μg/ml(r=0.9996)范围内线性关系良好,平均回收率分别为99.2%和99.5%.     

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.