RP—HPLC梯度洗脱法测定血塞通片中三七皂苷R1、人参皂苷Rb1及人参皂苷Rg1的含量

目的:用高效液相色谱梯度洗脱法同时检测血塞通片中三七皂苷R_1、人参皂苷Rb_1和人参皂苷Rg_1 3种皂苷的含量。方法:用Eclipse XDB—C_8分析柱;乙腈-水二元梯度洗脱;0—15 min(25:75—32:68),平衡5 min;流速1.0 mL·min~(-1);检测波长203 nm。结果:三七皂苷R1、人参皂苷Rg_1和人参皂苷Rb_1的线性范围分别为O.51-3.05,1.68—10.09,2.73—16.39μg。该方法回收率三七皂苷R_1为99.92%(RSD=0.70%)、人参皂苷Rg_1为98.93%(RSD=1.4%)、人参皂苷Rb_1为102.8%(RSD=0.81%)。结论:HPLC梯度洗脱法能将多种皂苷很好地分离检测,提高了时效,减少了误差,结果表明该方法准确可靠,重现性好,结果稳定。     

藤丹胶囊质量标准方法的改进

目的完善藤丹胶囊的质量标准。方法修订川芎、黄芪、三七的TLC方法、增加丹参、防己的TLC方法,建立HPLC法测定三七中人参皂苷Rg_1、人参皂苷Rb_1、三七皂苷R1的含量和丹参中丹酚酸B的含量测定。三七的含量测定:以Agilent 5 TC-C_(18)(250mm×4.6mm,5μm)为色谱柱;以乙腈为流动相A,以0.1%磷酸溶液为流动相B进行梯度洗脱;流速1.0m L/min;柱温:35℃;丹参的含量测定:以Agilent Extend C_(18)(250mm×4.6mm,5μm)为色谱柱;流动相:乙腈-1%甲酸溶液(20︰80);流速:1.0m L/min;柱温:35℃。结果三七皂苷R1进样量在1.1545~4.1562μg、人参皂苷Rg_1进样量在5.833~20.9988μg、人参皂苷Rb_1进样量在3.849~13.8564μg、丹酚酸B进样量在1.1~6.6μg范围内,与峰面积呈良好的线性关系,r=0.9998、r=0.9999、r=0.9996、r=0.9999;加样回收率分别为:平均回收率分别为98.39%、101.11%、101.11%,104.05%。结论完善后的质量标准可行,能有效控制藤丹胶囊的质量。     

HPLC法测定红药胶囊中三七皂苷R1及人参皂苷Rg1的含量

目的:建立红药胶囊中三七皂苷 R_1及人参皂苷 Rg_1的含量测定方法。方法:采用 Alltima—C_(18)(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%磷酸溶液(20:80),流述为1.0 mL·min~(-1),检测波长为203 nm;柱温为40℃,外标法测定。结果:三七皂苷 R_1和人参皂苷 Rg_1进样量分别在0.345～2.76μg(r=0.9999)和0.945～7.56μg(r=0.9999)范围内与峰面积呈良好线性关系;平均回收率(n=6)分别为98.6%和99.2%。结论:本法简便可靠,专属性强,可用于红药胶囊的质量检测。     

田七痛经胶囊检测方法的研究

目的:建立田匕痛经胶囊的质量控制方法。方法:采用 TLC 方法对田七痛经胶囊中的木香、川芎、延胡索进行定性鉴别;采用 HPLC 法,YWG C_(18)色谱柱(250 mm×4.6 mm,10μm),以乙腈-0.05%(v/v)磷酸溶液(100:400)为流动相,流速1 mL·min~(-1),检测波长203 nm,柱温为室温,进样量20μL,对田七痛经胶囊中的三七皂苷 R_1、人参皂苷 Rg_1和人参皂苷 Re 进行定性鉴别,并对人参皂苷 Rg_1进行含量测定。结果:木香、川芎、延胡索的薄层鉴别和三七皂苷 R_1、人参皂苷 Rg_1和人参皂苷Re 的 HPLC 鉴别专属性强,人参皂苷 Rg_1进样量在3.0～15.0μg范围内与峰面积呈良好的线性关系(r=1.000,n=5)。人参皂苷 Rg_1。平均回收率为99.1%,RSD=2.6%(n=5)。结论:本方法可准确地进行定性、定量,可用于控制田七痛经胶囊的质量。     

RP-HPLC法同时测定西洋参含片中4种成分

目的建立同时测定西洋参含片中人参皂苷Rg_1、人参皂苷Re、人参皂苷Rb_1及拟人参皂苷F11含量的RP-HPLC方法。方法色谱柱为Agilent TC-C18(250 mm×4.6 mm,5μm);流动相为0.5 mL·L~(-1)磷酸溶液(A)-乙腈(B),梯度洗脱;流速:1.0mL·min~(-1);检测波长:203nm;柱温:30℃。结果人参皂苷Rg_1和人参皂苷Re及人参皂苷Rb_1在2.5~500μg·mL~(-1)、拟人参皂苷F11在5.0~1 000μg·mL~(-1)范围内线性关系良好(r≥0.999 4);平均加样回收率均大于95.0%。结论该方法简便、准确,重复性好,可作为西洋参含片的质量控制方法。     

高效液相色谱-蒸发光散射测定三七中三七皂苷R1及人参皂苷Rg1、Re、Rb1的含量

目的:用 HPLC—ELSD 测定三七药材中三七皂苷 R_1及人参皂苷 Rg_1、Re、Rb_1的含量。方法:色谱柱为 Lichrospher NH_2柱(4.6 mm×250 mm,5μm),流动相为乙腈-水(80:20);漂移管温度为90℃,载气流速为2.1 L·min~(-1)。结果:三七皂苷 R_1及人参皂苷 Rg_1、Re、Rb_1分别在0.316～1.58μg、1.21～6.05μg、0.448～2.24μg及1.49～7.47μg呈良好线性关系;药材中4种成分的平均回收率(n=6)分别为102.2%(RSD=2.6%)、99.4%(RSD=2.2%)、101.8%(RSD=2.5%)及97.6%(RSD=2.4%)。结论:该方法简便、准确,分离效果好,无干扰,可用于三七药材的质量评价。     

搜风通胶囊中三七皂苷R_1、人参皂苷Rg_1和Rb_1的含量测定

目的建立以高效液相色谱法(HPLC)测定搜风通胶囊中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1含量的方法。方法采用色谱柱Hypersil ODS C18柱(4.6mm×250mm,5μm);流动相为乙腈(A)-水(B),进行梯度洗脱(0～12min,19%A,12～60min,19%～36%A),流速:1.0mL/min,柱温:30℃,检测波长:203nm。结果三七皂R1、人参皂苷Rg1和人参皂苷Rb1的线性范围分别为0.107～2.638μg(r=0.9998)、0.428～10.623μg(r=0.9999)和0.424～10.526μ(gr=0.9997);平均加样回收率分别为98.33%(RSD=1.16%)、98.22%(RSD=1.60%)和97.78%(RSD=0.98%)。结论本方法简便、准确、重现性好,可用于搜风通胶囊中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1含量的测定。     

HPLC—ELSD测定红参中人参皂苷Rg1、Re、Rb1含量

目的:用 HPLC-ELSD 测定红参中人参皂苷 Rg_1、Re、Rb_1含量。方法:采用 Agilent XDB-C_(18)柱(4.6 mm×150 mm,5 μm),柱温30℃;流动相为乙腈-水,梯度洗脱[0～24 min:乙腈-水(19.5:80.5);24～39 min:乙腈-水(30:70)],流速1.0 mL·min~(-1);漂移管温度98.8℃,载气流速2.7 L·min~(-1)。结果:人参皂苷 Rg_1、Re、Rb_1分别在1.08～6.48 μg、0.678～4.068 μg、1.024～6.144 μg范围内呈良好的线性关系。3种人参皂苷的平均回收率(n=5)分别为99.2%(RSD=1.3%),99.3%(RSD=2.4%),99.9%(RSD=1.9%)。结论:本方法灵敏、简便、准确。     

HPLC法同时测定注射用艾迪（冻干）中人参皂苷Rg1和人参皂苷Re的含量

目的:建立注射用艾迪(冻干)中人参皂苷Rg_1和人参皂苷Re的含量测定方法。方法:色谱柱为Hypersil C_(18)柱(250mm×4.6mm,5μm),流动相为乙腈-0.05%磷酸溶液(19∶81),流速为1.0mL·min~(-1),检测波长为203nm。结果:人参皂苷Rg_1浓度在20～200μg·mL~(-1),人参皂苷Re浓度在10～100μg·mL~(-1)范围内与峰面积呈良好的线性关系,相关系数分别为0.9997和0.9996;平均回收率分别为100.3%和97.6%(n=9)。结论:本法快速,准确,重复性好,可作为注射用艾迪(冻干)的质量控制方法。     

RP—HPLC测定人参各部位人参皂苷compound K的含量

目的:考察人参皂苷 compound K 是否存在于人参植物体中并测定其含量。方法:采用氯仿-甲醇(15∶1)超声提取,并用 Zorbax SB C_(18)色谱柱(4.6 mm×150 mm,5μm),以乙腈和水作为流动相进行二元梯度洗脱,流速为0.8 mL·min~(-1),检测波长为203 nm。结果:人参花和人参果中人参皂苷 compound K 的含量分别为0.02%和0.04%。人参皂苷 compound K 在0.523～10.45μg范围内呈良好的线性关系(r=0.9996),平均回收率为97.55%。在人参茎叶、鲜人参主根、红参芦头、红参主根、红参须根中未检出人参皂苷 compound K。结论:在人参植物体中存在人参皂苷 compound K。本方法简便、灵敏和准确,可作为人参皂苷 compound K 的有效分析方法。     

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.