反相高效液相色谱法测定维C银翘片中绿原酸的含量

目的:建立测定维C银翘片中绿原酸的反相高效液相色谱法.方法:采用CLC-ODS柱(6.0mm×250mm,5μm),以甲醇-水-冰醋酸(20∶80∶0.8)为流动相,流速为1.0ml·min-1,检测波长为326nm.结果:样品中绿原酸平均回收率为98.2%,RSD为1.59%,n=5;绿原酸在5～60μg·ml-1内,r=0.9998,峰面积与浓度线性关系良好.结论:绿原酸与其他成分能得到很好的分离.     

反相高效液相色谱法测定金银花合剂中的绿原酸含量

目的　建立一种用反相高效液相色谱法测定金银花合剂中绿原酸的含量。方法　以shim - packCLC -ODS (2 0 0mm× 4 .6mm ,5um )为色谱柱 ,用甲醇 -水 -冰醋酸 (35∶6 5∶0 .5 )作流动相 ,检测波长为 :32 7nm ,流速 :1 .0mL/min ,柱温 :常温 ,外标法定量。结果　绿原酸在 1 5 μg·mL-1 ～ 1 0 5 μg·mL-1 范围内呈现出良好的线性关系 ,(r =0 .9999) ,方法平均回收率为 :1 0 0 .2 5 %,RSD为 0 .4 8%(n =4 )。结论　该方法简便、快速 ,测定结果准确可靠 ,可用于金银花合剂的质量控制。     

HPLC法测定速克感冒片中阿司匹林、绿原酸的含量

目的建立速克感冒片中绿原酸和阿司匹林的含量测定方法。方法采用高效液相色谱法,色谱柱C18柱(250 mm×4.6mm,5μm),测定阿司匹林的流动相为甲醇-水-冰醋酸(26∶23∶1)、检测波长为280 nm。测定绿原酸的流动相为甲醇-水-冰醋酸(13∶87∶1)、检测波长为327nm。结果线性范围:阿司匹林30.65~490.4 mg.L-1(r2=0.999 6)、绿原酸5.4~108 mg.L-1(r2=0.999 9)。加样回收率:阿司匹林为99.55%,RSD为0.38%(n=6);绿原酸为98.78%,RSD为0.56%(n=6)。结论本方法操作简单、结果准确,可作为控制本品质量的方法。     

高效液相色谱法测定银翘感康胶囊中绿原酸的含量

目的:建立银翘感康胶囊中绿原酸的HPLC测定方法。方法:采用高效液相色谱法,用Shim-pack VP-ODS C18柱(250mm×4.6mm,5μm),以甲醇-水-冰醋酸-三乙胺(15∶85∶1∶0.3)为流动相,流速为1.0mL·min-1,检测波长为324nm。结果:绿原酸在5.12～153.60μg·mL-1呈良好的线性关系(r=0.9999),平均回收率为98.72%,RSD为0.46%。结论:所建方法准确可靠,操作简便,稳定性好,可用于银翘感康胶囊的质量控制。     

高效液相色谱法测定桑菊感冒片中绿原酸的含量

目的:建立HPLC法测定桑菊感冒片中绿原酸的含量。方法:采用高效液相色谱法,以Diamonsil C18(250mm×4.6mm,5μm)为分析柱;甲醇-水-冰醋酸-三乙胺(18∶85∶1∶0.3)为流动相;流速为1.0mL.min-1;检测波长为324nm。结果:绿原酸的线性范围为6.92～76.12mg.L-1(r=0.999 9)。平均回收率为99.9%;RSD为0.5%(n=9)。结论:该方法简便、快速、准确,适用于该制剂的质量控制。     

高效液相色谱法测定退黄洗剂中绿原酸含量

目的:建立退黄洗剂中绿原酸的含量测定方法。方法:采用HPLC法,色谱柱为DiamonsilC18(250mm×4.6mm,5μm);流动相为甲醇-水-冰醋酸-三乙胺(15∶350∶4∶1.2);检测波长为327nm。结果:绿原酸线性范围为21.08~210.8mg·L-1(r=0.9997),平均回收率为98.39%,RSD为1.15%。结论:方法准确可行,可用于该制剂的质量控制。     

速效止泻胶囊定性定量检测方法研究

目的:建立速效止泻胶囊的定性定量检测方法。方法:采用TLC法鉴别速效止泻胶囊中盐酸小檗碱和拳参;采用HPLC法测定处方中盐酸小檗碱含量及拳参中绿原酸含量。盐酸小檗碱色谱条件:依利特Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.05 mol·L-1磷酸二氢钾溶液-三乙胺(40∶60∶0.1)为流动相,流速1 mL·min-1,紫外检测波长346 nm,柱温为30℃;绿原酸色谱条件:依利特Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.01 mol·L-1磷酸二氢钾溶液-三乙胺-磷酸(7∶93∶0.4∶0.3)为流动相,流速1 mL·min-1,紫外检测波长327 nm,柱温为30℃。结果:盐酸小檗碱和拳参薄层色谱定性鉴别特征明显;盐酸小檗碱与绿原酸含量测定,分别在2.0～6.0μg(r=0.9992)和0.1～1.8μg(r=0.9999)线性关系良好;平均回收率(n=6)分别为99.2%和102.3%,RSD分别为0.77%和1.3%。结论:本法可准确地定性、定量,有效地控制速效止泻胶囊的质量。     

刺五加果TLC鉴别及原儿茶酸、绿原酸、金丝桃苷的含量测定

目的建立刺五加果的TLC定性鉴别法和原儿茶酸、绿原酸、金丝桃苷的HPLC色谱含量测定法。方法以金丝桃苷为对照品,采用氯仿-甲醇-水-冰醋酸(体积比为65∶35∶4∶1)为展开剂,在UV 254nm下检视,对刺五加果进行薄层色谱法定性鉴别。采用Hypersil ODS2柱(150mm×4.6mm,5μm),冰醋酸-水(体积比为1∶99)和甲醇-乙腈(体积比为1∶1)为流动相,在254nm检测波长下,以HPLC法测定刺五加果中原儿茶酸、绿原酸、金丝桃苷的含量。结果刺五加果薄层色谱中,金丝桃苷斑点清晰、分离度好。HPLC定量分析中,原儿茶酸、绿原酸、金丝桃苷线性范围分别为2.0~50.0mg·L-1(r=0.999 8)、8.0~200 mg·L-1(r=0.999 6)、2.0~50.0 mg·L-1(r=0.999 5),平均回收率分别为99.4%(RSD=2.7%)、100.9%(RSD=1.8%)和98.1%(RSD=2.4%)。结论该方法可用于刺五加果的质量控制。     

HPLC法测定感咳清颗粒中绿原酸的含量

目的:建立感咳清颗粒中绿原酸的含量测定方法.方法:采用RP-HPLC法,Kromasil C18色谱柱(150 mm×4.6 mm,5μm),用乙腈-0.4%磷酸(10∶90)为流动相,流速为1.0 mL·min-1,检测波长为327 nm.结果:在选定的实验条件下,绿原酸在0.15～0.75μg的范围内呈良好的线性关系,r=0.999 6,平均回收率98.77%,RSD为1.30%(n=6).结论:该方法操作简便,结果准确,可作为该制剂中绿原酸的含量测定方法.     

HPLC法测定蒲公英中绿原酸和咖啡酸的含量

目的建立HPLC法同时测定蒲公英中咖啡酸和绿原酸的含量。方法采用Agilent ZORBAX SB-C_(18)(250mm×4.6mm,5μm);流动相:甲醇-20mL·L~(-1)磷酸盐缓冲液(19∶81);检测波长:326nm;流速:1.0mL·min~(-1);柱温:30℃。结果绿原酸和咖啡酸质量浓度分别在1.152～23.040和2.524～50.480μg·mL~(-1)范围内线性关系良好,线性方程分别为y_1=102.9x_1+13.219(r_1=0.999 5),y_2=236.65x_2+29.535(r_2=0.999 6);平均回收率分别为97.59%和97.61%;RSD值分别为0.88%和0.95%。结论该方法专属性强,分离度好,稳定可靠,简便易行,可用于蒲公英药材中咖啡酸和绿原酸的含量测定。     

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.