HPLC法测定谷氨酸诺氟沙星注射液的有关物质及含量

目的 采用HPLC法测定谷氨酸诺氟沙星注射液的有关物质及含量.方法 采用ODS柱,以0.025 mol·L-1磷酸溶液(用三乙胺调节Ph值至3.0)-乙腈(84∶16)为流动相,检测波长为278 nm.谷氨酸诺氟沙星在18.8～93.9 mg·L-1范围内线性关系良好(r=0.999 8),检测限为0.298 ng,平均回收率为99.80%,RSD为0.59%.结果 在本文所设计的实验条件下,有关物质检查的专属性较好.在含量测定条件下,该方法的线性范围、回收率、精密度、重复性、耐用性及稳定性的考察结果都较满意.结论 采用HPLC法对谷氨酸诺氟沙星注射液的有关物质和含量进行测定具有专属性强,结果准确及操作简便等优点.     

高效液相色谱法测定谷氨酸诺氟沙星注射液含量

目的通过高效液相色谱法测定谷氨酸诺氟沙星注射液的含量并确定质量标准。方法采用高效液相色谱法,色谱柱为DiamonsilTMC18柱,以0.025mol/L磷酸溶液(用三乙胺调节pH值至3.0)-乙腈(84:16)为流动相,检测波长为278nm,理论板数按诺氟沙星计算应不低于2000,诺氟沙星峰与相邻杂质峰的分离度应符合规定。结果进样量在0.416-1.248μg线性关系良好,r=0.9994,平均加样回收率为99.6%,RSD=0.79%。结论本测定方法简便、准确、重复性好,可用于测定谷氨酸诺氟沙星注射液的含量,作为检测质量标准。     

HPLC法同时测定复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱

目的　建立一种快速、准确的高效液相色谱法同时测定诺氟沙星 ( NOR)和盐酸麻黄碱 ( EPH)的含量。 方法　使用 C1 8色谱柱 ,流动相为乙腈— 0 .1%磷酸 ( 15 :85 V/V) ,检测波长为 2 5 6nm。结果 　样品测定在 9min内完成。诺氟沙星在 10～ 60μg· ml- 1 浓度范围内 ,r=0 .9999,RSD= 0 .46% ,平均回收率为 99.91% ;盐酸麻黄碱在 2 5～ 12 5 μg· ml- 1浓度范围内 ,r=0 .9992 ,RSD=0 .5 1% ,平均回收率为 10 0 .0 3%。 结论 　方法可快速准确地检测复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱含量     

高效液相色谱法测定甲硝唑诺氟沙星栓的含量

建立甲硝唑诺氟沙星栓中甲硝唑、诺氟沙星含量的HPLC测定方法.色谱柱为SUNTEK Kromasil C18柱;流动相为0.025mol·L-1磷酸溶液(用三乙胺调节pH值至3.0±0.1)-乙腈(80:20),流速为1.0ml·min-1,检测波长为278nm,线性范围为甲硝唑2.5～20μg·ml-1,r=0.9999,诺氟沙星2.5～20μg·ml-1,r=0.9999,平均回收率甲硝唑为97.55%,RSD为0.6%,诺氟沙星为97.96%,RSD为0.8%.方法准确可靠,简单易行,适用于甲硝唑诺氟沙星栓中甲硝唑、诺氟沙星的含量测定.     

反相离子对色谱法测定诺氟沙星滴眼液中的诺氟沙星和有关物质

目的 :建立了一种反相离子对色谱法测定诺氟沙星滴眼液中的诺氟沙星和有关物质。方法 :用SpherisorbC18ODS柱 ,甲醇 0 .0 5mol·L-1磷酸盐缓冲液 0 .0 5mol·L-1四丁基溴化铵 (2 5∶75∶4,pH =2 .75 )为流动相 ,紫外检测波长为 2 80nm。结果 :诺氟沙星线性范围 :0 .12～ 1.0 0 μg ,r =0 .9994,平均回收率为 98.0 % ,RSD为 1.0 % (n =5 )。结论 :该法准确、快速、简便 ,可用于诺氟沙星滴眼液中的诺氟沙星的含量测定。     

高效液相色谱法测定复方甲硝唑栓中甲硝唑及诺氟沙星的含量

目的建立测定复方甲硝唑栓中甲硝唑及诺氟沙星含量的高效液相色谱法.方法采用Symmetry C18色谱柱(4.6 mm×150 mm,5μm),以乙腈-0.03 mol·L-1磷酸溶液(用三乙胺调节pH 3.0)(15;85)为流动相,流速为1.0 mL·min-1,检测波长为315 nm.结果甲硝唑及诺氟沙星在浓度范围内,峰面积与其浓度线性均关系良好(甲硝唑r=0.999 9,诺氟沙星r=1.000 0),平均回收率分别为100.64%和100.29%,精密度试验RSD分别为0.1%和0.2%,重复性试验RSD分别为1.5%和0.92%.结论该方法准确,简便,快速,专属性强,灵敏度高,适用于复方甲硝唑栓中甲硝唑及诺氟沙星的含量测定.     

高效液相色谱法测定甲诺参洗剂中甲硝唑及诺氟沙星的含量

目的:建立同时测定甲诺参洗剂中甲硝唑和诺氟沙星含量的高效液相色谱法.方法:采用Kromasil C 18 色谱柱(250 mm× 4.6 mm,5 μm),0.7%三乙胺(以磷酸调pH至 3.0 )-甲醇(200∶300)为流动相,流速为 1.0 mL·min -1 ,检测波长为290 nm.结果:甲硝唑在 20.0 ～ 150.0 mg·L -1 范围内,峰面积与其浓度线性关系良好(r= 0.999 9 ),平均回收率为 100.4% ,重复性试验RSD为 0.4% (n=5),检测限为 4.0 ×10 -3 μg;诺氟沙星在 10.0 ～ 75.0 mg·L -1 的范围内,峰面积与其浓度线性关系良好(r= 0.999 9 ),平均回收率为 98.6% ,重复性试验RSD为 0.5% (n=5),检测限为 2.0 ×10 -3 μg.结论:本法准确、简便、快速,具有专属性强,灵敏度高的特点,适用于含甲硝唑及诺氟沙星制剂的含量测定.     

鲎试验测定谷氨酸诺氟沙星氯化钠注射液中的细菌内毒素

目的建立快速的谷氨酸诺氟沙星氯化钠注射液的细菌内毒素检查法。方法用不同厂家的鲎试剂对不同批号的谷氨酸诺氟沙星氯化钠注射液分别进行干扰试验,考察确立谷氨酸诺氟沙星氯化钠注射液的内毒素检查法。结果将谷氨酸诺氟沙星氯化钠注射液稀释至0.8mg/ml可消除干扰作用。结论利用细菌内毒素检查法检查谷氨酸诺氟沙星氯化钠注射液中的内毒素可行。     

高效液相色谱法测定诺氟沙星滴眼液的含量

目的 　采用高效液相色谱法测定诺氟沙星滴眼液的含量。方法 　C1 8柱 (15 0× 4.6mm,5 μm) ,流动相为 0 .0 2 5 mol·L- 1磷酸溶液 (用三乙胺调节 p H值至 3 .0± 0 .1) -乙腈 (87∶ 13 ) ;流速 1.0 ml· min- 1 ;检测波长 2 78nm。结果 　诺氟沙星在 0 .1～ 1.0μg呈良好线性 (r=0 .9998) ,平均回收率 10 0 .0 %,RSD为 0 .5 %。 结论 　本法简便、快捷 ,结果准确 ,重现性好     

反相HPLC同时测定复方诺氟沙星滴眼液中诺氟沙星和地塞米松磷酸钠的含量及有关物质

目的 建立反相高效液相色谱法测定复方诺氟沙星滴眼液中诺氟沙星和地塞米松磷酸钠的含量及有关物质.方法 使用反相高效液相色谱法.用资生堂SHISEIDO C18(UG120,4.6mm×250mm,50m)色谱柱;以醋酸铵高氯酸钠溶液(取醋酸铵2.4g和高氯酸钠4.2g,用水900mL使溶解,用磷酸调pH值至2.5,再加水稀释至1000mL).乙腈-甲醇(68:22:10)为流动相;检测波长有关物质为278nm,地塞米松磷酸钠含量测定为242nm,诺氟沙星含量测定为278nm.结果 诺氟沙星的最低检测限为0.5ng;诺氟沙星在12.1～120.8μg/mL、地塞米松磷酸钠在2.1-21.2μg/mL的范围内浓度与峰面积呈良好的线性关系,线性回归方程分别为A=69068C-1619(r=1.000)和A=25580C+382(r=1.000);两组分的回收率分别为100.01%和99.87%,相对标准偏差(RSD)为0.4%和0.4%.结论 本方法灵敏、准确、专属性强可用于测定复方诺氟沙星滴眼液中两组分的含量和有关物质.     

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.

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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.