RP-HPLC法测定蒙药森登-4汤中栀子苷、槲皮素和没食子酸的含量

目的建立测定蒙药森登-4汤中栀子苷、槲皮素和没食子酸的高效液相色谱方法。方法栀子苷的测定条件为:Hypersil C18 ODS(250.0 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-水(体积比为13.5∶86.5),流速为0.8 mL.min-1,检测波长为238 nm。槲皮素的测定条件为:Century SIL C18 BDS(250.0 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水-磷酸(体积比为60.00∶40.00∶0.02),流速为0.8 mL.min-1,检测波长为360 nm;没食子酸的测定条件为:Century SIL C18 BDS(250.0 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-水-磷酸(体积比为5.00∶95.00∶0.02),流速为0.80 mL.min-1,检测波长为272 nm。结果在各自的色谱条件下,栀子苷、槲皮素和没食子酸质量浓度与峰面积具有良好的线性关系。平均回收质量分数分别为:栀子苷96.9%(RSD=1.9%,n=6);槲皮素97.1%(RSD=2.3%,n=6);没食子酸98.7%(RSD=1.7%,n=6)。结论该方法可作为该制剂的含量测定方法。     

UV和HPLC法分别测定板栗种仁中总多糖和没食子酸的含量

目的研究测定板栗种仁中总多糖及没食子酸的含量的方法。方法总多糖含量测定:以葡萄糖为对照品,采用分光光度法,于620 nm处测定;没食子酸含量测定:采用HPLC法,色谱柱为Diamonsil ODS C18柱(200 mm×4.6 mm,5μm),流动相为甲醇-水-磷酸(体积比为4.0∶96.0∶0.1),检测波长为273 nm,流速为1 mL.min-1。结果葡萄糖的质量在45.0~225.0μg(r=0.9999)、没食子酸的质量在0.044~0.440μg(r=0.9998)内线性关系良好,总多糖和没食子酸的平均回收率分别为97.7%(RSD为0.8%,n=6)和101.3%(RSD为1.2%,n=6)。结论建立的方法可为板栗的质量控制提供依据。     

高效液相色谱法测定石榴皮中没食子酸的含量

目的测定石榴皮中没食子酸的含量。方法采用高效液相色谱法,Zorbax-C18色谱柱,流动相水-二甲基甲酰胺-冰醋酸(99.82-0.15-0.03),检测波长270nm,流速1mL.m in-1,柱温为室温。结果在0.081~0.811μg.mL-1范围内,没食子酸峰面积(Y)与其进样量(X)呈良好的线性关系(r=0.9999),平均日内、日间RSD为1.01%和1.60%(n=6),不同浓度的平均回收率为98.35%,RSD=1.63%(n=6)。结论该法快速简便,稳定可靠,专属性强。     

高效液相色谱法测定维吾尔药制剂西帕依固龈液中没食子酸含量

目的建立测定西帕依固龈液中没食子酸含量的高效液相色谱法。方法色谱柱为VP-ODS柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.025%磷酸溶液(4∶96),流速为1 mL/min,检测波长为270 nm,柱温为25℃,进样量为10μL,分析方法为外标法。结果没食子酸质量浓度在10.6～106.0μg/mL范围内与峰面积线性关系良好(r=0.999 6),方法精密度的RSD为0.42%(n=5),平均回收率为99.12%,RSD为1.34%(n=6)。结论该方法简便、准确、测得结果稳定,重现性好,可作为该制剂中没食子酸的含量测定方法。     

RP-HPLC法同时测定桂枝茯苓胶囊中3种成分的含量

目的建立RP-HPLC法同时测定桂枝茯苓胶囊中没食子酸、白芍苷和芍药苷含量。方法色谱柱:大连中汇达C18柱(4.6 mm×250 mm,5μm),流动相:乙腈-体积分数为0.1%的磷酸溶液,梯度洗脱,流速:1.0 mL.min-1,检测波长:230 nm,柱温:40℃。结果没食子酸、白芍苷和芍药苷的线性分别为0.69~6.87 mg.L-1(r=0.999 6)、0.88~8.80 mg.L-1(r=0.999 6)和2.00~20.00 mg.L-1(r=0.999 5)。平均回收率:没食子酸为99.7%(RSD=1.0%,n=9)、白芍苷为101.5%(RSD=1.5%,n=9)、芍药苷为100.0%(RSD=0.7%,n=9)。结论此方法可为桂枝茯苓胶囊的质量控制提供方法。     

RP-HPLC法测定茶色素中没食子酸和咖啡因的含量

目的:建立以反相高效液相色谱法测定茶色素中没食子酸和咖啡因含量的方法。方法:色谱柱为Novapak ODS分析柱(250mm×4.6mm,5.4μm),流动相为乙酸-甲醇-N,N-二甲基甲酰胺-水(2:3:35:160),检测波长为280nm,流速为1.0mL.min-1。结果:没食子酸、咖啡因的检测浓度分别在8.16～81.60、2.84～28.40μg.mL-1范围内与各自峰面积积分值呈良好线性关系;没食子酸的平均回收率为99.8%(RSD=0.5%,n=6),咖啡因的平均回收率为99.9%(RSD=0.6%,n=6)。结论:本方法快速、灵敏、准确,可用于茶色素的质量控制。     

高效液相色谱法测定景天三七胶囊中没食子酸的含量

目的建立景天三七胶囊中没食子酸含量的测定方法。方法采用HPLC法,色谱柱为Dia-monsil C18(200 mm×4.6 mm,5μm),流动相为甲醇-0.6%磷酸溶液(12∶88),检测波长271 nm,流速1.0 mL/min,柱温40℃。结果没食子酸线性范围为160.1~800.5 ng(r=0.999 9);平均回收率为99.05%,RSD=0.88%(n=6)。结论所用方法简便、快速、准确。     

HPLC测定益肝除湿合剂中的没食子酸

目的 采用HPLC法测定益肝除湿合剂中没食子酸的含量.方法 采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-乙腈-0.1％磷酸溶液(5∶6∶89)为流动相,检测波长264.5 nm,流速1 mL· min-1,柱温30℃.结果 0.01～2.54 μg没食子酸与峰面积的线性关系良好(r=0.9997),平均回收率为99.32％,RSD =0.90％(n=6).结论 所用方法简便、易控、准确可靠,可用于益肝除湿合剂的质量控制.     

反相高效液相色谱法测定血安胶囊中没食子酸含量

目的建立测定血安胶囊中没食子酸含量的反相高效液相色谱法。方法色谱柱采用Hypersil ODS2柱(200mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸溶液(3∶97),检测波长为214nm,流速为1.0mL/min。结果没食子酸进样量在0.0211~0.211μg范围内与峰面积呈良好线性关系(R2=1),平均回收率为99.28%,RSD=1.73%(n=6)。结论该方法简便、快速、结果准确、重复性好,可用于血安胶囊中没食子酸含量的测定。     

HPLC法测定痔速宁片中没食子酸的含量

目的　建立高效液相色谱法测定痔速宁片中没食子酸含量的方法。方法　采用C18ODS反相色谱柱(4.6mm×2 5 0mm ,5 μm) ,流动相为甲醇-冰醋酸-N ,N -二甲基酰胺-水(2∶1∶4 0∶15 7) ,检测波长2 75nm ,流速0 .5mL·min-1,柱温2 5℃。结果　没食子酸的线性范围为0 .4 1～2 .0 7μg(r =0 .9997) ;平均回收率为98.6 0 % (RSD =1.2 1% ,n =6 )。结论　本法简便、准确、灵敏度高、重现性好,可用于该制剂中没食子酸的含量测定。     

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.     

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.