HPLC-ELSD测定酸枣仁合剂中酸枣仁皂苷A的含量

目的 建立酸枣仁合剂中酸枣仁皂苷A的含量测定方法.方法 应用高效液相色谱-蒸发光散射检测器(HPLCELSD),色谱柱:Hypersil ODS-2C18(250 mm×4.6 mm,5μm);流动相:甲醇-水(60:40),测定酸枣仁合剂中酸枣仁皂苷A的含量.结果 平均回收率为99.09%(RSD=3.05%).结论 本方法简便,重现性良好,可作为酸枣仁合剂的质量控制方法.     

酸枣仁合剂的薄层鉴别及酸枣仁皂苷A的含量测定

目的:建立酸枣仁合剂的鉴别和含量测定方法.方法:采用TLC法和HPLC法.结果:TLC法鉴别酸枣仁合剂中知母、茯苓和川芎等药材;HPLC测定酸枣仁皂苷A的含量,酸枣仁皂苷A在0.55～1.1 mg/mL范围内线形关系良好(r=0.9997),平均加样回收率为100.45%,RSD为1.30%.结论:鉴别重复性好、专属性强,含量测定方法简便,准确.     

睡安口服液中酸枣仁皂苷A和酸枣仁皂苷B的含量测定

目的:为睡安口服液建立专属性酸枣仁皂苷A和酸枣仁皂苷B的含量测定方法.方法: 采用HPLC法测定,色谱柱为Kromasil C18柱.结果: 睡安口服液中酸枣仁皂苷A在0.928～4.604μg范围内线性关系良好, 酸枣仁皂苷B在0.468～2.340μg范围内有良好线性关系,回收率分别为97.6%,97.5%,RSD分别为0.9%、1.9%.结论: HPLC法可做为睡安口服液中酸枣仁皂苷A和酸枣仁皂苷B的含量测定方法.     

HPLC-ELSD测定酸枣仁汤不同配伍情况下酸枣仁皂苷A和B的含量

目的:建立HPLC-ELSD测定酸枣仁汤不同配伍情况下各组方中酸枣仁皂苷A和B含量的方法。方法:采用GraceBrava C18-BDS(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-水(B)为流动相进行梯度洗脱,流速1.0 mL.min-1,柱温25℃;ELSD参数:漂移管温度100℃,载气流速2.9 L.min-1。结果:酸枣仁皂苷A和B浓度分别在49.50～900.0"g.mL-1和20.40～407.2"g.mL-1范围内呈良好的线性关系;平均加样回收率(n=6)分别为101.9%(RSD=2.3%)和100.7%(RSD=3.0%)。结论:酸枣仁与其他药味配伍后,酸枣仁汤中酸枣仁皂苷A和B的含量发生一定变化,其他药味的存在不同程度地影响其溶出。     

HPLC-DAD-ELSD法同时测定酸枣仁中斯皮诺素、酸枣仁皂苷A和B的含量

目的:建立同时测定酸枣仁中斯皮诺素、酸枣仁皂苷A和B含量的HPLC-DAD-ELSD方法。方法:采用Grace BravaC18-BDS(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-水(B)为流动相进行梯度洗脱,流速1.0 mL.min-1,二极管阵列检测器的检测波长为335 nm,蒸发光散射检测器的漂移管温度为100℃,载气流速为2.9 L.min-1,柱温为25℃,。结果:斯皮诺素、酸枣仁皂苷A和B的线性范围分别为59.40~594.0μg.mL-1(r=0.9996),49.50~900.0μg.mL-1(r=0.9998),20.36~407.2μg.mL-1(r=0.9999);平均加样回收率(n=6)分别为96.9%(RSD=1.8%),101.2%(RSD=2.5%),100.3%(RSD=2.9%)。结论:该方法准确、可靠,在同一色谱条件下实现多指标成分的同时测定,为酸枣仁的全面质量评价提供参考。     

水提过程中粉碎对酸枣仁中酸枣仁皂苷A溶出的影响

目的研究粉碎与未粉碎酸枣仁所含有效成分酸枣仁皂苷A在水提取过程中的溶出是否有差异。方法采用高效液相色谱法测定粉碎与未粉碎酸枣仁的酸枣仁皂苷A含量。色谱枉为Agilent C18柱（250mm×4．6mm，5μm），流动相为甲醇-水（65：35），流速为1．0mL／min，蒸发光散射检测器漂移管温度110℃，载气流量2．4L／min。结果在未粉碎的酸枣仁水提样品中未检测出酸枣仁皂苷A，而粉碎后的酸枣仁水提样品的酸枣仁皂苷A含量为0．0090％。结论临床应用时，酸枣仁宜粉碎。     

神牡胶囊中酸枣仁皂苷A的含量测定

目的建立神牡胶囊中酸枣仁皂苷A的含量测定方法。方法采用HPLC法,色谱柱:kromasil C18柱;流动相:乙腈-水(33∶67),蒸发光散射检测器;流速:1.0 mL.min-1;气流:2.5mL.min-1;漂移管温度110℃。结果酸枣仁皂苷A对照品进样量在0.24～6.0μg范围内呈良好线性关系(r=0.999 0),平均加样回收率为98.0%,RSD为3.1%(n=7)。结论该法可以方便、准确的测定神牡胶囊中酸枣仁皂苷A的含量。     

高效液相色谱法-蒸发光散射检测器测定安神胶囊中酸枣仁皂苷A和B的含量

目的建立安神胶囊中酸枣仁皂苷A和B含量的测定方法。方法应用高效液相色谱法-蒸发光散射检测器(HPLC-ELSD),以YMC-PackODS柱(200mm×4.6mm,5μm)为色谱柱,甲醇-水-冰醋酸(70∶30∶2)为流动相,流速是1.0mL/min,柱温:25℃;漂移管温度95℃,气体流速1.05L/min。结果酸枣仁皂苷A线性范围是2.47～12.34μg,r=0.9999,平均回收率为99.3%,RSD=1.89%(n=6);酸枣仁皂苷B线性范围是1.34～6.70μg,r=0.9999,平均回收率为99.3%,RSD=1.5%(n=6)。结论该方法快速简便,重现性良好,可用于测定安神胶囊中酸枣仁皂苷A和B的含量。     

酸枣仁皂苷提取物的制备与酸枣仁皂苷A和B的含量测定

目的优化酸枣仁总皂苷的大孔吸附树脂纯化工艺;并进一步建立RP-HPLC法同时测定酸枣仁皂苷提取物中酸枣仁皂苷A和B的含量。方法采用单因素方法对纯化工艺条件进行优化,得到酸枣仁皂苷提取物,进而建立RP-HPLC法对酸枣仁提取物中酸枣仁皂苷A和B进行含量测定。结果最佳纯化工艺为:采用AB-8型大孔吸附树脂进行纯化,上样吸附时间为1.5 h,洗脱流速为1.0 mL.min-1,体积分数为70%的乙醇溶液洗脱160 mL。采用此纯化方法得到的酸枣仁皂苷提取物中皂苷的质量分数为52%,测得其酸枣仁皂苷A和B的含量质量分数分别为2.298%和0.789%。酸枣仁皂苷提取物中酸枣仁皂苷A和B的质量浓度分别在14.7～293.0 mg.L-1(r=0.999 7,n=6)、7.2～144.0 mg.L-1(r=0.999 6,n=6)内与峰面积呈良好线性关系;平均回收率(n=9)分别为103.7%、101.9%。结论该工艺稳定可行且提取物中皂苷含量高,具有广泛的应用前景;建立的RP-HPLC法可为酸枣仁皂苷提取物质量标准的建立提供一定依据。     

酸枣仁皂苷E的结构鉴定酸枣仁皂苷E的结构鉴定

目的研究酸枣仁(Ziziphus jujuba Mill var. spinosa)的化学成分。方法用各种色谱方法分离酸枣仁的化学成分,用波谱(IR,UV,MS,NMR)方法鉴定结构。结果从酸枣的干燥种子中分离得到7个化合物,分别鉴定为酸枣仁皂苷E(1,jujuboside E),酸枣仁皂苷B(2,jujuboside B)及酸枣仁皂苷A(3,jujuboside A),白桦酯酸(4,betulic acid),硬脂酸(5,stearic acid),蔗糖(6,sucrose)和肌苷(7,inosine)。结论化合物1为新化合物,5,6和7为首次从酸枣仁中获得。     

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.

     

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.     

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.     

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.     

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.