高效液相色谱法测定六味地黄胶囊中熊果酸含量

目的建立测定六味地黄胶囊熊果酸含量的高效液相色谱法。方法色谱柱为Phenomenex C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-0.5%醋酸铵溶液(67∶12∶21),流速为1.0 mL/min,检测波长为210 nm,柱温为30℃。结果熊果酸进样量的线性范围为1.041～5.204μg,r=0.999 9(n=6),平均加样回收率为98.01%,RSD=0.36%(n=6)。结论该法简便、快速、准确,可用于六味地黄胶囊的质量控制。     

HPLC法同时测定毛建草中齐墩果酸和熊果酸的含量

目的建立毛建草中齐墩果酸和熊果酸的高效液相色谱测定方法。方法采用ODS柱,流动相为乙腈-甲醇-水-醋酸铵(70∶14∶16∶0.05),检测波长210nm。结果齐墩果酸在0.196～3.920μg范围内线性关系良好,熊果酸在0.512～12.800μg范围内线性关系良好;该法回收率齐墩果酸为99.5%,熊果酸为100.6%;齐墩果酸RSD为2.0%,熊果酸RSD为2.2%(n=6)。结论为毛建草的含量测定提供了一种快速、准确的方法,为蒙药植物资源的进一步开发提供了依据。     

HPLC-ELSD法测定枇杷叶中齐墩果酸和熊果酸的含量

目的建立枇杷叶中熊果酸和齐墩果酸含量的HPLC-ELSD测定法。方法采用C18色谱柱(250mm×4.6mm,5μm),以甲醇-水-冰乙酸-三乙胺(90∶10∶0.03∶0.06)为流动相,流速为1.0mL·min-1,柱温为30℃,蒸发光散射检测器飘移管温度为100℃。结果熊果酸在0.244~7.335μg范围内线性关系良好(r=0.9997,n=6),回收率为96.0%;齐墩果酸在0.118~3.525μg范围内线性关系良好(r=0.9998,n=6),回收率为95.2%。结论该方法测定准确,重现性好,可用于枇杷叶的质量控制。     

HPLC法同时测定5种常见中药材中齐墩果酸和熊果酸的含量

目的:建立测定含有齐墩果酸与熊果酸中药材的方法,并测定这些中药材中齐墩果酸与熊果酸的含量,为其品质评价提供依据。方法:采用高效液相色谱法。色谱柱为Welch Materials Ultimate XB C18(250mm×4.6mm,5μm),检测波长为210nm,流动相为甲醇-0.1%磷酸-三乙胺(86∶14∶0.05,V/V/V),流速为0.6mL·min-1。结果:齐墩果酸进样量在0.330～3.300μg范围内与峰面积积分值呈良好线性关系(r=0.9998),平均加样回收率为98.26%,RSD=0.47%(n=6);熊果酸进样量在0.390～3.900μg范围内与峰面积积分值呈良好线性关系(r=0.9994),平均加样回收率为97.98%,RSD=0.50%(n=6)。结论:本方法简便、准确、重复性好,可为含有齐墩果酸与熊果酸中药材的质量控制提供方法参考,且本试验数据可为这些中药材的质量评价提供科学依据。     

HPLC测定复方大红袍止血片中熊果酸的含量

目的建立复方大红袍止血片中熊果酸的含量测定方法。方法采用高效液相色谱法。用Kromasil C18色谱柱(150 mm×4.6 mm,5μm);流动相为甲醇-水-磷酸(85∶15∶0.2);流速0.5 ml.min-1;柱温40℃。结果熊果酸在0.2012~1.6096μg范围内线性关系良好(r=0.9999),平均回收率为98.4%,方法精密度RSD=1.8%。结论所用方法简便可行、重复性好,适用于复方大红袍止血片的质量控制。     

RP-HPLC法同时测定夏枯草中3种三萜酸的含量

目的:建立同时测定夏枯草中齐墩果酸、熊果酸和2α,3α-二羟基-12-烯-28-熊果酸含量的方法。方法:采用反相高效液相色谱法。色谱柱为Diamonsil C18(2)柱(250mm×4.6mm,5μm),流动相为甲醇-1%醋酸铵水溶液(85∶15,V/V),流速为1.0mL·min-1,检测波长为210nm,柱温为30℃。结果:齐墩果酸、熊果酸和2α,3α-二羟基-12-烯-28-熊果酸的进样量分别在0.1～2.0μg(r=0.9998)、0.3～6.0μg(r=0.9995)和0.04～0.80μg(r=0.9997)范围内与各自峰面积积分值呈良好的线性关系;三者平均加样回收率分别为99.0%、98.6%和98.7%,RSD分别为0.9%、1.4%和1.1%(n均为9)。结论:该方法准确、简便、重复性好,可用于夏枯草的质量控制。     

薄层扫描法测定小儿健胃消食颗粒中熊果酸的含量

目的:建立小儿健胃消食颗粒中熊果酸含量的测定方法。方法:采用薄层扫描法,展开剂为氯仿-丙酮-冰醋酸(18∶2∶0.2),显色方法为10%硫酸乙醇溶液,于110℃下烘至斑点显清晰的紫红色,扫描方法为双波长反射式锯齿扫描,测定波长为520nm,参比波长为700nm,线性参数Sx=3,狭缝大小为0.4mm×0.4mm。结果:熊果酸进样量在2μg～10μg范围内与峰面积积分值线性关系良好(r=0.9996),平均回收率为97.8%(RSD=1.4%)。结论:本方法可用于小儿健胃消食颗粒的质量控制。     

HPLC法测定不同产地夏枯草中熊果酸的含量

目的:建立以高效液相色谱法测定夏枯草中熊果酸含量的方法,并检测不同产地夏枯草中熊果酸的含量。方法:色谱柱为ZorbaxSBC18(150mm×4.6mm,5μm),流动相为乙腈-磷酸盐缓冲液(pH7.6)=45∶55,检测波长为210nm,流速为1.0mL·min-1。结果:熊果酸进样量在0.1115～1.7840μg范围内与峰面积积分值呈良好的线性关系(r=0.9992);平均回收率为99.93%,RSD=0.77%(n=6)。不同产地夏枯草中熊果酸的含量在0.08%～0.18%之间。结论:不同产地夏枯草中熊果酸含量差异很大。本方法简便、准确、重现性好,可用于夏枯草的质量控制。     

RP-HPLC法同时测定蒙药复方菖蒲四味中熊果酸与齐墩果酸的含量

目的:建立同时测定蒙药复方菖蒲四味中熊果酸与齐墩果酸含量的方法。方法:采用反相高效液相色谱法。色谱柱为Diamosil C18(250mm×4.6mm,5μm),流动相为甲醇-乙腈-0.2%冰醋酸水溶液(56∶28∶16),流速为1.0mL·min-1,检测波长为215nm,柱温为30℃,进样量为20μL。结果:熊果酸、齐墩果酸的进样量分别在0.9264～9.2640μg(r=0.9999)、0.8656～8.6560μg(r=0.9999)范围内与各自峰面积积分值呈良好的线性关系;平均加样回收率分别为98.40%、99.29%,RSD分别为2.04%、1.44%(n=6)。结论:本法准确、简便、重复性好,可为蒙药复方菖蒲四味的质量控制提供依据。     

HPLC法测定岗梅中熊果酸和齐墩果酸的含量

目的:建立岗梅中熊果酸和齐墩果酸的含量测定方法。方法:采用高效液相色谱法。色谱柱为Thermo-C18,流动相为甲醇-乙腈-0.1%冰醋酸(83∶5∶12,V/V/V),流速为0.7 ml/min,柱温为30℃,检测波长为210 nm,进样量为10μl。结果:熊果酸和齐墩果酸的进样量分别在0.200 4~4.008μg(r=0.999 8)、0.100 9~2.018μg(r=0.999 6)范围内与各自峰面积呈良好的线性关系;精密度、稳定性、重复性试验的RSD<2%;熊果酸和齐墩果酸的平均加样回收率分别为98.85%、99.44%,RSD分别为1.88%、1.83%(n均为6)。结论:该方法准确、灵敏,可为岗梅的质量控制提供参考。     

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.

---

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.