HPLC法测定盐酸苯达莫司汀含量及有关物质

目的:建立盐酸苯达莫司汀含量及有关物质的分析方法.方法:采用色谱柱:C18(4.6 mm×250 mm,5 μm);流动相:十二烷基硫酸钠溶液(取十二烷基硫酸钠0.5 g置1000 mL水中使溶解,用磷酸调节pH值至4.0)-乙腈 (105∶95);检测波长:234 nm.结果:在选定的色谱条件下,有关物质与主药分离效果好,盐酸苯达莫司汀在84.91 μg～424.6 μg·mL-1范围内线性关系良好(r=0.9999).结论:方法可用于盐酸苯达莫司汀含量及有关物质的测定.     

HPLC法测定盐酸多巴胺的有关物质

目的:建立测定盐酸多巴胺有关物质的方法。方法:采用Nucleosil C18柱(100mm×4.6mm,5μm);流动相:0.005mol/L十二烷基硫酸钠-乙腈-冰醋酸-0.1mol/L乙二胺四醋酸二钠(700∶300∶10∶2);检测波长:280nm。结果:盐酸多巴胺的线性范围为1～11μg/ml,线性回归方程为Y=10755X-350.92,r=0.9999(n=6)。最低检测限为10.08ng。结论:实验证明该法简便快捷,能准确地测定盐酸多巴胺有关物质。     

氯硝柳胺中有关物质检查方法的研究

目的 建立氯硝柳胺中有关物质的检测方法。方法 采用高效液相色谱法(HPLC)：Diamonsil(C18柱4.6×250mm，5μm)，乙腈：缓冲液(每1000ml中含磷酸二氢钾2g，磷酸氢二钠1g，四正丁基硫酸氢铵2g)=3∶2为流动相，流速为1ml/min，检测波长为230nm，柱温为室温。结果 本法可检出氯硝柳胺...     

吡哌酸有关物质检查方法的研究

目的:采用HPLC法测定吡哌酸有关物质。方法:采用XDS-C18(150 mm×4.6 mm,5μm)色谱柱,流动相为枸橼酸癸烷磺酸钠溶液(取枸橼酸5.7 g、癸烷磺酸钠1.7 g,加水溶解并稀释至1 000 ml)-乙腈-甲醇(60∶20∶20),流速:1 ml/min,检测波长:275 nm,柱温:30℃,进样量:20μl。结果:吡哌酸在0.062 7～3.760 8μg/ml浓度范围内线性关系良好(r=1.000 0),最小检出限为0.04%。结论:本方法专属性强、灵敏度高、准确度和重复性好,方法简便,可作为吡哌酸有关物质的检测方法。     

梯度洗脱HPLC法测定盐酸平阳霉素及注射药物中的有关物质

目的 建立梯度洗脱HPLC法测定盐酸平阳霉素及注射用盐酸平阳霉素中的有关物质.方法 采用C18(150mm×4.6mm,5μm)色谱柱,己烷磺酸钠溶液(己烷磺酸钠7.53g与乙二胺四乙酸二钠3.72g以0.08mol/L乙酸溶液溶解并稀释至1000ml,用氨溶液调节pH为4.3)为流动相A,甲醇:乙腈(70:30)为流动相B,梯度洗脱,流速1.0ml/min,检测波长254nm,柱温30℃.结果 盐酸平阳霉素溶液在10～500μg/ml范围内,溶液浓度与峰面积呈良好线性关系,r=0.9999;最低检测浓度1μg/ml.结论 本法可用于测定盐酸平阳霉素及注射用盐酸平阳霉素中的有关物质.     

HPLC测定盐酸洛美利嗪胶囊的含量及有关物质

目的建立盐酸洛美利嗪胶囊的含量测定及有关物质检查方法。方法采用高效液相色谱法,色谱柱为Diamonsil-ODS柱(4.6 mm×150 mm,5μm),以乙腈-0.001 mol·L-1十二烷基硫酸钠溶液(60∶40)为流动相,流速1.0 mL·min-1,柱温35℃,波长225 nm。结果盐酸洛美利嗪与各主要杂质及强制破坏产生的降解产物的杂质峰均分离良好,盐酸洛美利嗪在17.04～153.40μg·mL-1内与峰面积呈良好线性关系,r=1.000,回收率为99.8%(RSD=1.12%,n=9),供试品溶液在24 h内稳定。结论本法专属性强,结果准确,方法灵敏可靠,可用于盐酸洛美利嗪的含量测定和有关物质检查。     

HPLC法测定溴丙胺太林片的含量和有关物质

目的:建立HPLC法测定溴丙胺太林片含量和有关物质的方法.方法:色谱柱:Venusil XBP C8(150mm×4.6mm,5μm);流动相:乙腈-磷酸盐缓冲液(取十二烷基硫酸钠17.3g,氢氧化钠5.0g,加水1000ml溶解,用磷酸调节pH至3.5±0.05,加水稀释至2000ml)(54:46);检测波长:254nm.结果:溴丙胺太林在0.003～3.000mg·ml-1范围内线性关系良好(r=1.0000);平均回收率为100.2%,RSD=1.1%;各杂质峰的分离度均达到要求.结论:本测定方法准确、灵敏、专属性高,可作为溴丙胺太林片的含量测定和有关物质检查方法.     

高效液相色谱法测定炎可宁片中盐酸小檗碱的含量

目的 应用HPLC法测定炎可宁片中盐酸小檗碱的含量.方法 色谱柱为Kromasil C18柱(4.6 mm×250 mm,5 μm);流动相:乙腈-水(1:1)(每1 000 ml中加入磷酸二氢钾3.4 g和十二烷基硫酸钠1.7 g);流速1.0 ml·min-1;柱温:30℃;检测波长265 nm.取样品定量加甲醇-...     

HPLC法测定头孢羟氨苄及其有关物质含量

目的建立头孢羟氨苄有关物质的HPLC分析方法。方法采用ODS柱(Polaris250mm×4.6mm,5μm),以0.05mol/L磷酸盐缓冲液(用10mol/L氢氧化钾调节pH值为5.5)-乙腈(96∶4)为流动相,流速为0.7ml/min,检测波长为230nm。结果头孢羟氨苄、有关物质α-对羟基苯甘氨酸、7-氨基去乙酰氧基头孢烷酸(7-ADCA)的线性范围分别为0.125～1.0mg/ml(r=0.9997)、0.312～20μg/ml(r=0.9999)、0.312～20μg/ml(r=0.9999)。结论本方法可用于头孢羟氨苄及其有关物质含量的测定,方法准确、灵敏、简便。     

RP-HPLC测定氢溴酸右美沙芬原料中的有关物质

目的 采用RP-HPLC法测定氢溴酸右美沙芬原料中的有关物质.方法 采用Luna Scx 100 A色谱柱(250 mm×4.6mm,5 μm);取3.4 g丁二酸二辛酯磺酸钠溶于550 ml乙腈和450 ml水的混合液中,加入0.56 g硝酸铵,以冰醋酸调pH3为流动相;流速为1.0 ml·min-1;检测波长280 nm;柱温35℃.结果 氢溴酸右美沙芬与3-甲氧基吗啡氢溴酸盐能达到基线分离,方法的精密度、准确性、灵敏度、专属性均能满足要求.结论 所建方法可用于测定氢溴酸右美沙芬中的有关物质.     

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.

---

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.