反相高效液相色谱法测定注射用细辛脑的含量

目的：建立反相高效液相色谱法(RP HPLC)测定注射用细辛脑的含量。方法：采用C18柱(4.6 mm×200 mm，5 μm)，以甲醇 水(60∶40)为流动相，流速1.0 mL·min 1，紫外检测波长313 nm。结果：平均回收率99.93%，RSD＝0.69%(n＝9)，细辛脑在10～50 μg·mL 1范围内浓度与峰面积呈良好线性关系，r＝0.999 9。结论：该方法简便、准确，可以有效控制该制剂的质量。     

高效液相色谱法测定磷酸川芎嗪葡萄糖注射液中川芎嗪的含量

目的：探讨用高效液相色谱(HPLC)法测定磷酸川芎嗪葡萄糖注射液中川芎嗪的含量的方法。方法：采用Spherisorb C18色谱柱，以乙腈 0.02 mol·L 1磷酸二氢钾溶液(35∶65)为流动相；检测波长295 nm。结果：磷酸川芎嗪在12～28 μg·mL 1浓度范围内，浓度与峰面积呈良好的线性关系。平均回收率99.2%，RSD＝1.2%。结论：采用HPLC法测定磷酸川芎嗪含量灵敏性高，准确性和专属性好。     

反相高效液相色谱法测定新生化冲剂中阿魏酸含量

目的：建立测定新生化冲剂中阿魏酸含量的方法。方法：采用反相高效液相色谱(RP HPLC)法，以ODS C18色谱柱分离，以水(水中含1.0%冰醋酸)∶乙腈∶甲醇＝70∶0.6∶30为流动相，流速为1.0 mL·min 1，检测波长320 nm。结果：线性范围5.4～86.4 μg·mL 1，r＝0.998 7，测得平均回收率99.7%，RSD＝0.49%。结论：反相高效液相色谱法高效、快速、灵敏，可作为新生化冲剂质量控制的有效方法。     

高效液相色谱法测定胃灵颗粒中甘草酸含量

目的：建立测定胃灵颗粒中甘草酸含量的方法。方法：采用高效液相色谱法(HPLC)，Hyersil C18柱(250 mm×4.6 mm，5 μm)；流动相：甲醇 0.2 mol·L 1醋酸铵溶液 冰醋酸(66∶33∶1)；检测波长：254 nm。结果：甘草酸在7.444～37.220 μg·mL 1范围内线性关系良好，r＝0.999 5，回收率为98.58%，RSD＝0.65 %。结论：该方法简便、准确、可控，可作为该产品的质量控制方法。     

复方乳酸左氧氟沙星滴眼液的制备与含量测定

目的：研究复方乳酸左氧氟沙星滴眼液的制备及含量测定方法。方法：用紫外分光光度法和化学分析法对乳酸左氧氟沙星和地塞米松磷酸钠进行定性鉴别，用反相高效液相色谱法(RP HPLC)进行含量测定。以ODS C18分析柱(4.6 mm×250 mm，5 μm)为固定相，0.2%三乙胺水溶液(用磷酸调pH至2.7) 乙腈(68∶32)为流动相，检测波长240 nm，流速1.0 mL·min 1。结果：乳酸左氧氟沙星的线性范围12～60 μg·mL 1，r＝0.999 9，平均回收率99.66%，RSD＝1.9%(n＝5)。地塞米松磷酸钠的线性范围3～15 μg·mL 1，r＝0.999 1，平均回收率100.8%，RSD＝1.8%(n＝5)。结论：该制剂处方设计合理，制备方法可行，灵敏度高，测定结果准确，精密度良好。     

磷酸川芎嗪氯化钠注射液的制备与质量控制

目的：制备磷酸川芎嗪氯化钠注射液，并对其质量进行控制。方法：磷酸川芎嗪1.0 g，氯化钠9.0 g，纯化水溶解并加至1 000 mL定容制备磷酸川芎嗪氯化钠注射液。采用高效液相色谱法测定磷酸川芎嗪含量，银量法测定氯化钠含量。结果：磷酸川芎嗪在20.0～200.0 μg· mL 1浓度范围内线性关系良好(r＝0.999 9)，平均回收率100.13%，RSD＝0.56%(n＝9)；氯化钠平均回收率100.27%，RSD＝0.39%(n＝9)。结论：该制剂处方合理，制备工艺简便，质量易于控制。     

反相离子对色谱法测定复方双氯芬酸钠注射液的含量

目的建立反相离子对色谱法（RPIC）同时测定复方双氯芬酸钠注射液中盐酸利多卡因和双氯芬酸钠的含量。方法色谱柱：Alltech C18（150 mm×4.6 mm，5 μm）；流动相：0.05 mol·L 1磷酸二氢钠缓冲液（用磷酸调pH值2.8） 乙睛（40∶60）配制的4 mmol·L 1的庚烷磺酸钠溶液；流速1.0 mL·min 1；检测波长：213 nm；柱温：室温。结果盐酸利多卡因在20～120 μg·mL 1范围内线性关系良好（r＝0.999 9），平均回收率99.9 %，重复性实验RSD ＝0.3%(n＝6)；双氯芬酸钠在75～450 μg·mL 1范围内线性关系良好，平均回收率99.5%，重复性实验RSD为 0.5%(n＝6)。结论该法简便准确，可用于复方双氯芬酸钠注射液的含量测定。     

高效液相色谱法测定六味健胃颗粒剂中芍药苷的含量

目的：建立六味健胃颗粒剂中芍药苷含量的高效液相色谱(HPLC)测定法。方法：采用Hypersil ODS(4.0 mm×125 mm，5 μm)色谱柱，流动相为乙腈 水(25∶75)；检测波长230 nm。结果：浓度在0.512～8.192 μg·mL 1范围线性关系良好，r＝0.999 9。平均回收率100.45%，RSD＝1.85%(n＝5)。结论：HPLC测定六味健胃颗粒剂中芍药苷的含量方法简便、快速、准确。     

当归注射液中阿魏酸的含量测定

目的:以反相高效液相色谱(RP HPLC)法测定当归静脉注射液中阿魏酸的含量.方法:采用CLC ODS色谱柱(5 μm,150 mm×6 mm),流动相:甲醇 水 冰醋酸(70∶30∶1),流速:0.8 mL•min 1,检测波长:323 nm.结果:阿魏酸在4.4～26.4 μg• mL 1范围内线性关系良好,r＝0.999 1,平均回收率98.96%(RDS＝1.96%).结论:该法简便、易行,可用于当归静脉注射液中阿魏酸的含量测定.     

反相高效液相色谱法测定氯氮平片的含量

目的：建立反相高效液相色谱法(RP HPLC)测定氯氮平片含量的方法。方法：采用Techsphere ODS分析柱(4.6 mm×250.0 mm，5 μm)和Spherisorb ODS(4.6 mm×10.0 mm，5 μm)保护柱，流动相为甲醇 乙腈 水 三乙胺(32∶28∶40∶0.4，V/V)，醋酸调pH值为4.50，流速为1.0 mL·min 1，检测波长为254 nm，对氯氮平片剂进行含量检测，并采用紫外分光光度法进行对比实验。结果：氯氮平的保留时间为6.54 min，其浓度在5～30 μg·mL 1范围内线性关系良好(r＝0.999 7，n＝6)，平均回收率为100.96%，RSD为0.83%(n＝5)。结论：该法简单、结果准确、重复性好，可作为氯氮平片剂含量测定方法。     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.     

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.