HPLC法测定丹栀逍遥丸中芍药苷的含量

选用 Hgpersil- ODS(5μm,1 2 5mm× 4mm)乙腈 -水 -磷酸 (1 5∶ 85∶ 0 .1 )为流动相 ,检测波长 2 30 nm。流速为 0 .7ml· min- 1 。结果 :线性范围 1 .0～5.0μg,r=0 .9995,平均回收率为 99.0 % ,RSD=1 .2 %。本法简便、灵敏、准确。     

高效液相法测可乐定贴片的释放度

目的　建立一种采用高效液相色谱检测可乐定贴片的释放度的方法。方法　采用 KP1 0 0 - SC1 8色谱柱 (2 5 mm× 4 .6 mm ) ,流动相为乙腈∶水∶三乙胺 =5 0∶ 5 0∶ 0 .0 5 (用稀磷酸调节至 p H4 .8) ,UV检测波长为 2 0 0nm。结果　该法平均回收率为 1 0 0 .4 3% ,RSD为 1 .4 3% (n=5 )。结论　该法操作简便、快速     

反相高效液相色谱法测定金银花合剂中的绿原酸含量

目的　建立一种用反相高效液相色谱法测定金银花合剂中绿原酸的含量。方法　以shim - packCLC -ODS (2 0 0mm× 4 .6mm ,5um )为色谱柱 ,用甲醇 -水 -冰醋酸 (35∶6 5∶0 .5 )作流动相 ,检测波长为 :32 7nm ,流速 :1 .0mL/min ,柱温 :常温 ,外标法定量。结果　绿原酸在 1 5 μg·mL-1 ～ 1 0 5 μg·mL-1 范围内呈现出良好的线性关系 ,(r =0 .9999) ,方法平均回收率为 :1 0 0 .2 5 %,RSD为 0 .4 8%(n =4 )。结论　该方法简便、快速 ,测定结果准确可靠 ,可用于金银花合剂的质量控制。     

高效液相色谱手性流动相添加剂法拆分麻黄碱对映体

目的　建立HPLC手性流动相添加剂法拆分麻黄碱对映体。方法　选用AgilentEclipseXDB -C8色谱柱 (4 .6mm× 2 5 0mm ,5 μm) ,LabAllianceC8保护柱 (4 .6mm× 10mm) ;流动相为水 -甲醇 -乙腈 (4 9∶4 6∶5 ) ,其中含 9.0mmol·L-1β -CD、0 .2 %磷酸且pH 5 .30 ,流速为 0 .8ml·min-1;检测波长 2 5 4nm ;进量样 2 0 μl;柱温为室温。 结果　建立了 β -环糊精手性流动相添加剂法拆分麻黄碱对映体的方法。结论　该方法分离度好、简便 ,比手性固定相经济     

HPLC法测定茵栀黄软胶囊中黄芩苷、栀子苷和绿原酸的含量

目的测定茵栀黄软胶囊中的 3种有效成分 ,黄芩苷、栀子苷、绿原酸的含量。方法HPLC法 ,Irregular HC18(2 5 0 . 0mm× 4 6mm ,10 μm)色谱柱。黄芩苷流动相 :甲醇 水 磷酸 (V∶V∶V =4 7. 0∶5 .3 0∶0. 2 ) ,流速 :1 0mL·min-1,检测波长 :2 80nm ;栀子苷流动相 :乙睛 水 (V∶V =15∶85 ) ,流速 :1 0mL·min-1,检测波长 :2 38nm ;绿原酸流动相 :乙睛 磷酸溶液 (w =0 . 4 % )(V∶V =13∶87) ,流速 :1 0mL·min-1,检测波长 :32 7nm。结果黄芩苷在 2 7 5～ 137 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =6 4. 83× 10 4ρ - 1 6. 96× 10 .5 ,r =0 . 9998,平均回收率为 99 4 6 % (RSD =1 0 1% ) ;栀子苷在 16 .5～ 82 . 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =8 794× 10 .5ρ - 4 . 116× 10 2 ,r =0 . 9999,平均回收率为 10 0 . 37% (RSD =1 4 .0 % ) ;绿原酸在 2 4～ 12 0mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =2 4 88× 10 4ρ - 9 2 4 4× 10 4,r =0 9999,平均回收率为 99 38%(RSD =1. 89% )。结论测定方法可用于茵栀黄软胶囊的质量控制。     

HPLC法测定依那普利的血药浓度

目的建立高效液相色谱法测定马来酸依那普利的血药浓度。方法采用SpherisorbC18柱(2 5 0mm× 4 6mm ,5 μm) ,流动相 :乙腈 -甲醇 -水 -磷酸 -三乙胺 (V∶V∶V∶V∶V =5 0∶2 3 0∶2 75∶0 3∶0 1 ) ,流速 :0 9mL·min-1,检测波长 2 1 5nm。结果马来酸依那普利的血药浓度在 1 0～3 0 0 μg·L-1内 ,与其峰面积有良好的线性关系 (r=0 9942 )。方法回收率为 1 0 1 1 % ,日内精密度小于 5 5 % ,日间精密度小于 5 4%。结论该方法可用于马来酸依那普利的药代动力学及生物利用度研究。用此法测定了家犬口服国产依那普利片后的血药浓度并计算了药代动力学参数     

反相高效液相色谱法测定风湿骨痛颗粒中甘草酸的含量

目的　研究风湿骨痛颗粒中甘草酸的定量分析方法。方法　采用高效液相色谱法。色谱柱。shim packclc ODS(15 0mm× 4 6mm ) ;流动相 :甲醇 -水 -冰醋酸 -三乙胺(6 0∶38∶1∶0 3) ;检测波长 :2 5 0nm ;柱温 :30℃ ;结果　甘草酸含量测定的线性范围为 16 4 2～ 82 10 μg(r =0 9999,n =5 ) ,平均加样回收率为 98 0 2 % ,RSD为 1 4 2 %。结论　该方法简便、快速准确 ,可作为该制剂的质量控制方法     

高效液相色谱法测定卡托普利片含量

目的　建立卡托普利片含量的高效液相测定法。 方法 　利用高效液相色谱法测定 ,选用 Kromasil C1 8柱 ,( 5μm,2 0 0 mm× 4.6mm) ;流动相 :0 .0 1%磷酸二氢钠溶液 -乙腈 -甲醇 ( 66∶ 17∶ 17)流速 1.0 m L· min- 1 ;检测波长 :2 15 nm;柱温 5 0℃。没食子酸丙脂作内标物质。结果 　线性范围为 2 5μg· m L- 1～ 75μg· m L - 1 ;方法回收率为 10 0 .4%,RSD=0 .83 %( n=9)。 结论 　该方法简便 ,灵敏 ,准确     

高效液相色谱法测定参芍胶囊芍药苷的含量

目的　建立反相高效液相色谱法测定参芍胶囊中芍药苷的含量。方法 　本品以甲醇 -水 (1∶ 1)超声振荡提取 ,提取物滤过、离心后 ,进行高效液相色谱分析。色谱柱 Extend-C1 8(5 μm.4.6× 2 5 0 mm) ;流动相为甲醇 -水 -乙腈 (10∶ 75∶ 15 ) ;流速 :1.0 ml·min- 1 ;柱温 :3 0℃ ;检测波长 :2 3 0 mm。结果 　平均加样回收率为 99.0 3～ 99.5 4% ,RSD为 1.5～ 2 .1% (n=6)。 结论 　实验结果表明 ,该法操作简便、重现性好 ,可作为样品的检测方法     

离子对色谱法测定心脑安颗粒中葛根素含量

目的 :建立心脑安颗粒葛根素的含量测定方法。方法 :离子对色谱法 ,ODSC18柱 ,4 .6mm× 15 0mm(5 μm) ;流动相 :甲醇 水 (2 0∶80 ) ,内含 0 .0 0 2 4 %磷酸和 0 .0 0 12 %三乙胺 ;检测波长 :2 5 4nm ;流速 :1.0ml·min-1结果 :色谱分离良好 ,在 0 .0 2～0 .6 4 μg范围内成线性关系 ,Y =- 0 .12 5 +2 .6 4 2× 10 -5X ,r =0 .9999,平均回收率为 97.3% ,RSD为 1.5 8%。结论 :本方法简单、快速、准确 ,适合该制剂快速定量分析     

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.