HPLC法测定不同生长期女贞子中红景天苷的含量

目的:建立以高效液相色谱法测定不同生长期女贞子中红景天苷含量的方法。方法:色谱柱为InertsilODS-3C18(250mm×4.6mm,5μm),流动相为乙腈-水(13∶87),流速为1mL·min-1,检测波长为222nm,柱温为室温,进样量为20μL。结果:红景天苷检测浓度在11.9～238μg·mL-1范围内与峰面积积分值呈良好线性关系(r=0.9999);平均回收率为99.1%,RSD=1.2%(n=6)。红景天苷在女贞子幼果中(8月)含量最高并随生长期延长逐渐下降,到12月果实成熟时含量最低。结论:不同采收期女贞子中红景天苷的含量不同,故应适时采收。     

HPLC-荧光检测法测定雪域红景天口服液中红景天苷的含量

目的建立高效液相色谱法测定雪域红景天口服液中红景天苷的含量。方法以ShimpackODS柱(4.6mm×250mm,5μm)为分析柱;甲醇-水(16∶84)为流动相;荧光检测波长λex=220nm,λem=315nm。结果红景天苷在进样量0.084~0.420μg范围内呈良好的线性关系(r=0.9998);日间RSD=2.11%;平均加样回收率为98.89%。结论该法灵敏、准确、重复性好,可用于雪域红景天口服液中红景天苷的含量测定。     

RP-HPLC法测定大花红景天和长鞭红景天中红景天苷的含量

目的:建立测定大花红景天和长鞭红景天中红景天苷含量的方法。方法:采用反相高效液相色谱法。色谱柱为OPH RP-ODS C18(250mm×4.6mm,5μm),流动相为50mmol·L-1磷酸盐缓冲液(以氢氧化钠调pH值在7.0左右)-甲醇(90∶10),流速为1.0mL·min-1,柱温为室温,检测波长为253nm,进样量为10μL。结果:红景天苷的检测浓度在62.5～1000.0μg·mL-1范围内与峰面积积分值呈良好线性关系(r=0.9997);平均加样回收率为97.59%,RSD=1.71(n=6)。大花红景天中含有红景天苷,含量与等级呈线性关系;长鞭红景天含红景天苷较少或没有,不可作为其替代品。结论:本方法准确、灵敏、专属性强,可作为红景天药材中红景天苷的含量测定方法。     

高效液相色谱法测定肿瘤清胶囊中红景天苷的含量

目的:测定肿瘤清胶囊中红景天苷的含量.方法:采用高效液相色谱法.色谱柱为Kromasil C18柱(250 mm×4.6 mm,5 μm);甲醇-水-冰醋酸(20∶80∶1)为流动相,流速为1.0 mL·min-1;检测波长225 nm.结果:红景天苷在0.2～2.0 μg范围内具有良好线性关系,平均回收率为97.51%,RSD为1.32%.结论:该法可用于肿瘤清胶囊中红景天苷的含量测定.     

RP-HPLC法同时测定红景天口服液中红景天苷和酪醇的含量

目的建立反相高效液相色谱法同时测定红景天口服液中红景天苷和酪醇的含量。方法采用Kromasil C18柱(250 mm×4.6 mm,5μm);甲醇-水(体积比为20∶80)为流动相;柱温:30℃;检测波长:275 nm;流速:1.0 mL.min-1。结果红景天苷和酪醇分别在0.048~0.960 g.L-1(r=0.999 9,n=6)和0.013~0.390 g.L-1(r=1.000 0,n=6)内线性关系良好;平均回收率(n=9)分别为95.5%(RSD=1.3%)和95.2%(RSD=1.6%)。结论本方法可用于红景天口服液的质量控制。     

HPLC法测定复方红景天胶囊中红景天苷的含量

目的建立复方红景天胶囊中红景天苷的含量测定方法。方法样品采用甲醇超声提取的方法制备。色谱条件采用Shim-Pack ODS柱(150 mm×4.6 mm5,μm),甲醇-水(10∶90)为流动相,检测波长为223 nm。结果红景天苷浓度在9.61～96.08 mg.L-1范围内与峰面积值呈良好的线性关系(r=0.999 9)。回收率为97.34%,RSD=1.02%(n=6)。结论该法准确、可靠、稳定,可作为复方红景天胶囊的定量分析方法。     

柱层析预处理RP-HPLC法测定女贞子中红景天苷的含量

目的:建立女贞子中红景天苷含量测定的RP-HPLC法。方法:样品溶液经大孔树脂和聚酰胺柱层析纯化,采用Hypersil C18色谱柱(4.6 mm×150 mm,5μm),流动相为甲醇∶水(20∶80),流速0.4 mL/min,检测波长220 nm。结果:红景天苷在1~80μg/mL范围内线性关系良好(r=0.999 9),高、中、低浓度(40、10、5μg/mL)加样回收率分别为(101.4±1.52)%(、95.6±1.45)%、(100.5±2.18)%(n=5)。浓度为80、40、10μg/mL的红景天苷日内RSD分别为0.28%、0.17%、0.48%(n=5);日间RSD分别为0.56%、0.06%、0.12%(n=5)。稳定性的RSD=1.64%,表明红景天苷在24 h内稳定。应用该法测定女贞子中红景天苷的含量为0.718 mg/g。结论:本法简便、快捷、准确,适用于女贞子中红景天苷的含量测定。     

HPLC法测定复方红景天口含片中红景天苷和酪醇的含量

目的:建立测定复方红景天口含片中红景天苷和酪醇含量的方法。方法:采用高效液相色谱法。色谱柱为AgilentTC-C18(250mm×4.6mm,5μm),流动相为乙腈-水(8.5∶91.5),流速为1.0mL·min-1,检测波长为275nm。结果:红景天苷、酪醇的进样量分别在0.642～5.136μg(r=0.9997)、3.600～36.000μg(r=0.9991)范围内与各自峰面积积分值呈良好的线性关系;平均回收率分别为100.29%、99.46%,RSD分别为1.69%、2.25%(n=9)。结论:本方法简便、快速、重复性好,可用于复方红景天口含片的质量控制。     

RP-HPLC法测定5种红景天中红景天苷的含量

目的比较不同种及不同产地野生和种植的红景天中红景天苷和出膏率。方法采用Kro-masil C18色谱柱(5.0μm,4.6 mm×150.0 mm);以水-乙腈-磷酸(体积比为93.0∶7.0∶0.2)为流动相,流速为1.20 mL.min-1,柱温为30℃,检测波长为223 nm,进样10μL。结果红景天苷在12~60 mg.L-1内峰面积与对照品的质量浓度呈良好线性关系,回归方程为A=1.2 850ρ×104+7.648×103,r=0.999 8,其平均回收率为98.2%,RSD为2.4%(n=6)。结论为红景天药材的质量控制提供理论依据,红景天药材的质量与红景天种类、产地及野生或种植有一定关系。     

反相高效液相色谱法测定大花红景天及其混淆品中红景天苷的含量

目的建立RP-HPLC测定市场上大花红景天及其混淆品中红景天苷含量的方法。方法色谱柱为Phe-nomenex C18（250 mm×4.60 mm,5μm）,流动相为甲醇-水（15∶85）,等度洗脱,流速为1.0 mL.min-1,检测波长为223 nm,柱温为25℃。结果红景天苷在62.5～1 000μg.mL-1与峰面积线性关系良好（r=0.999 7,n=5）,平均加样回收率为100.1%,RSD为0.40%（n=6）。结论本方法简便、准确、重复性强,可用于市面上大花红景天及其混淆品中红景天苷的含量测定。     

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.