RP-HPLC法同时测定复方甘草酸苷片中三组分的含量

目的：建立高效液相色谱法同时测定复方甘草酸苷片中甘草酸单铵盐、甘氨酸和蛋氨酸的含量。方法：采用Diamonsil C18色谱柱（150mm×4.6mm,5μm）,流动相为乙腈-0.01mol·L^-1磷酸溶液（40：60）,流速1.0mL·min^-1,甘草酸单铵的检测波长为257nm,甘氨酸和蛋氨酸的检测波长为262nm。结果：甘草酸单铵盐、甘氨酸和蛋氨酸浓度分别在50.52～505.20μg·mL^-1、10.6～106.0μg·mL^-1、10.4～104.0μg·mL^-1范围内呈良好的线性关系;平均回收率分别为（100.32±1.35）%、（101.02±1.80）%和（100.75±1.86）%,RSD分别为1.35%、1.78%和1.85%（n=9）。结论：本法可用于同时测定复方甘草酸苷片中甘草酸单铵盐、甘氨酸和蛋氨酸的含量,方法简便,结果准确。     

HPLC法同时测定升麻葛根汤中四种有效成分的含量

目的：建立HPLC法同时测定升麻葛根汤中4种有效成分的含量.方法：采用Diamonsil C18色谱柱（250mm×4.6mm,5μm）,流动相：甲醇-乙腈-[1.6%冰醋酸的0.1 mol·L-1醋酸铵溶液]（12：7：81）,流速：1.0 ml·min-1,检测波长：320mm.结果：咖啡酸的线性范围为0.2～4 mg·L-1（r=0.999 6）,平均回收率为104.0%,RSD为0.59% 葛根素的线性范围为10～200 mg·L-1（r=0.999 5）,平均回收率为99.8%,RSD为0.63% 阿魏酸的线性范围为1～20 mg·L-1（r=0.999 5）,平均回收率为102.8%,RSD为0.96% 异阿魏酸的线性范围为2～40 mg·L-1（r=0.999 6）,平均回收率为98.O%,RSD为1.37%（n=9）.结论：方法简便、快捷、重复性好,可用于该汤剂的质量控制.     

HPLC测定感康片中对乙酰氨基酚、咖啡因和扑尔敏的含量

目的 建立同时测定感康片中对乙酰氨基酚、咖啡因和扑尔敏含量的方法.方法 采用HPLC法.Kromasil-C18柱(150 mm×4.6 mm,5 μm),乙腈-0.05 mol·L-1磷酸二氢钾溶液-三乙胺(10:90:0.2)为流动相,流速1.0 ml·min-1,检测波长222 nm.结果 对乙酰氨基酚的线性范围为120.0～320.0 μg·ml-1(r=0.9998),咖啡因的线性范围为7.2～19.2 μg·ml-1(r=0.9999),扑尔敏的线性范围为0.96～2.56 μg·ml-1(r=0.9999).平均回收率分别为99.4%、100%、99.1%(n=6).结论 所建方法可同时分离3种成分,分离效果好,灵敏度高,重复性好,准确可靠.     

RP-HPLC法测定氯霉素滴眼液中氯霉素及二醇物的含量

目的:测定氯霉素滴眼液中氯霉素和二醇物的含量.方法:采用RP-HPLC法.色谱系统:色谱柱:Kromasil ODS-1(250×4.6mm)流动相为水-甲醇-冰醋酸(55:45:0.1)[1],流速约为1ml·min-1,检测波长为278nm.结果:氯霉素与二醇物的平均回收率分别为100.6%、100.8%,RSD值分别为0.23%、1.49%.氟霉素线性范围为12.5μg·ml-1～300μg·ml-1,二醇物线性范围为1μg·ml-1～24μg·ml-1.结论:该法快速,简单,准确.可作为该制剂的质量控制标准.     

顶空气相色谱法测定左乙拉西坦中有机溶剂残留量

目的建立左乙拉西坦中有机溶剂残留量的顶空气相色谱分析方法.方法选用大口径HP-快速GC残留溶剂柱为分离柱,FID检测器,外标法进行定量,并对分离条件、顶空平衡温度、平衡时间对残留有机溶剂测定的影响进行了研究.结果二氯甲烷、乙酸乙酯、甲苯的线性范围分别为0.133～1.326 μg·mL-1(r=0.999 7),4.330～43.296 μg·mL-1(r=1.000 0),0.009～0.087 μg·mL-1(r=0.999 7);平均回收率范围99.70%～102.46%,精密度RSD(n=6)为1.79%～3.05%;检测限分别为0.008,0.005,0.001 μg·mL-1.结论该方法快速、灵敏、准确.     

梯度洗脱HPLC法同时测定双黄连口服液中绿原酸和黄芩苷含量

目的建立梯度洗脱HPLC法同时测定双黄连口服液(金银花,黄芩)中绿原酸和黄芩苷含量的方法.方法采用LUNAC18(2)色谱柱,乙腈-0.4%磷酸溶液为流动相(梯度洗脱),流速为0.9 ml·min-1,检测波长为318 nm.结果绿原酸线性范围为0.8～6.4 g·L-1,平均回收率为99.3%,RSD=1.3%;黄芩苷线性范围为 9.16～73.33 g·L-1,平均回收率为99.6%,RSD=1.5%.结论该方法简便、可靠、准确,可用于该制剂的质量控制.     

毛细管气相色谱法测定复方双辛喷雾剂含量

目的:建立以气相色谱法测定复方双辛喷雾剂中芳樟醇、甲基丁香酚及薄荷脑含量的方法.方法:以HP-5(0.32μm×30 m)弹性石英毛细管柱为色谱柱,采用外标法,对芳樟醇、甲基丁香酚及薄荷脑进行含量测定.结果:芳樟醇的线性范围为0.1811～1.086 7 mg·mL-1(r=0.999 4),回收率为100.63%;薄荷脑的线性范围为0.302 1～1.812 6 mg·mL-1(r=0.999 3),回收率为101.39%;甲基丁香酚的线性范围为0.266 4～1.598 4 mg·mL-1(r=0.999 2),回收率为99.01%.结论:本方法快速、准确,可用于本制剂的质量控制.     

毛细管气相色谱法测定复方薄荷脑滴鼻液中薄荷脑和樟脑含量

目的:建立GC法测定复方薄荷脑滴鼻液中薄荷脑和樟脑含量的方法.方法:采用SE-54弹性毛细管柱程序升温的方法测定.结果:薄荷脑线性范围为64.68～323.40 μg·L-1,平均回收率为98.0%,RSD为1.1%;樟脑线性范围为67.32～336.60μg·L-1,平均回收率为99.3%,RSD为1.4%.结论:该方法准确、可靠,可用于该制剂的质量控制.     

RP-HPLC法测定舒喘平胶囊中3个主要成分的含量

目的:建立反相高效液相色谱法测定舒喘平胶囊中二羟丙茶碱、盐酸去氯羟嗪、盐酸溴己新3个主要成分的含量.方法:用碱性处理的十八烷基键合硅胶(BDS)为填充柱,甲醇-水(95:5)为流动相,检测波长 240 nm.结果:二羟丙茶碱线性范围20.90～62.70 μg·mL-1,回收率99.6%,RSD为0.17%;盐酸去氯羟嗪线性范围6.40～19.20 μg·mL-1,回收率99.7%,RSD为0.54%;盐酸溴已新线性范围1.64～4.99 μg·mL-1,回收率100.0%,RSD为0.34%.结论:本法较简便,准确可靠,可作为舒喘平胶囊的质量控制方法.     

HPLC同时测定新复霜中氯霉素和倍他米松的含量

目的　建立新复霜中氯霉素和倍他米松的含量测定方法。方法　采用HPLC法 ,色谱柱为 μBondapakC18(10 μm ,3.9mm×30 .0mm) ,流动相为甲醇 - 0 .0 2 5mol·L-1NaH2 PO4(6 5∶35 ) ,检测波长 2 4 0nm ,流速 1 2ml·min-1,柱温 4 5℃ ,灵敏度 0 .0 2AUFS。结果　氯霉素的线性范围为 2 0 0 .0～ 5 0 0 .0mg·L-1,平均回收率为 10 .3 2 % (RSD为 0 . 83%～ 2 .17% ) ;倍他米松的线性范围为2 1.0～ 5 2 .5mg·L-1,平均回收率为 10 0 .8% (RSD为 1.11%～ 2 .6 4 % )。结论　所用方法简便、准确 ,适合新复霜的质量控制。     

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.