高效液相色谱法同时测定心脑健胶囊中表没食子儿茶素没食子酸酯和咖啡因的含量

目的建立测定心脑健胶囊中表没食子儿茶素没食子酸酯和咖啡因含量的高效液相色谱法。方法采用HypersilODSC18（250mm×4．6mm，5μm）色谱柱，流动相为0．04mol／L枸橼酸溶液-N，N二甲基甲酰胺-四氢呋哺（45：8：2），检测波长为278nm，流速为1．0ml／min，柱温为25℃。结果表没食子儿茶素没食子酸酯在0．408～4．08μg具有良好的线性关系，回归方程为：A=105．2C＋1210，r=0．9999。平均回收率98．59％，重现性（RSD）为0．78％。咖啡因在10．1～202ng具有良好的线性关系，回归方程为：A=-353．0C＋1442，r=0．9999。平均回收率98．71％，RSD为0．65％。结论该方法操作简单，重现性好，适用于心脑健胶囊中表没食子儿茶素没食子酸酯和咖啡因的含量测定。     

HPLC指纹图谱结合化学计量学分析不同企业心脑健胶囊(片)的差异

目的 建立心脑健胶囊(片)质量评价方法,比较不同企业心脑健胶囊(片)的质量差异。方法 将中国药典2020年版一部心脑健胶囊项下特征图谱转化为指纹图谱,并进行方法学考察。与对照品进行比较,确定特征峰成分。测定3个厂家的21批产品,通过相似度分析其指纹图谱的异同,进一步使用聚类分析和主成分分析进行模式识别。结果 3家企业之间心脑健胶囊(片)指纹图谱存在差异,聚类分析和主成分分析结果基本一致,样品按厂家各自聚为一类,其中峰10(表没食子儿茶素没食子酸酯),13(没食子酸儿茶素没食子酸酯)、16(表儿茶素没食子酸酯)等特征峰对指纹图谱影响较大。在企业H样品中表没食子儿茶素没食子酸酯含量较低,仅为企业N样品中相应成分含量的60.08%,而没食子酸儿茶素没食子酸酯含量较高。在企业S样品中没食子酸儿茶素没食子酸酯含量较低,为企业N样品中相应成分含量的42.47%,而表儿茶素没食子酸酯含量相对较高。另外,各企业样品所含主要成分的比例均不相同。结论 化学计量学辅助的HPLC指纹图谱具有简便、客观、可数字化的优点,可直观地区别不同企业心脑健胶囊(片)成分及其比例的差异。     

武当地区及其他产地茶叶中咖啡因和表没食子儿茶素没食子酸酯的含量测定

目的:采用HPLC法测定武当地区不同品种茶叶及其他地区茶叶的咖啡因和表没食子儿茶素没食子酸酯的含量。方法:以Luna-C18柱(250 mm×4.6 mm,5μm)为色谱柱,流动相为乙腈-0.2%磷酸水溶液,梯度洗脱,流速为0.75 ml·min^-1,检测波长为272 nm,柱温为25℃。结果:咖啡因和表没食子儿茶素没食子酸酯的线性范围分别为10.21~102.10μg·ml^-1(r=0.9994)、16.21~162.10μg·ml-1(r=0.9991),平均回收率分别为98.67%(RSD=1.86%,n=6),98.19%(RSD=2.28%,n=6)。结论:该方法用于武当地区及其他地区茶叶的咖啡因及表没食子儿茶素没食子酸酯含量的快速测定,具有简便、稳定性好、准确度高等特点,可以作为茶叶中咖啡因及表没食子儿茶素没食子酸酯含量的测定。     

反相高效液相色谱法测定心脑肾康胶囊中表没食子儿茶素没食子酸酯含量

目的建立测定心脑肾康胶囊的反相高效液相色谱法。方法采用芬兰产C18柱(5μm,4.6×150mm),0.04mol.L-1枸橼酸-N,N-二甲基甲酰胺-四氢呋喃(55∶8∶2)为流动相,流速:1.0mL.m in-1,检测波长:280nm,柱温:35℃,峰面积外标法定量。结果表没食子儿茶素没食子酸酯(EGCG)在0.24~1.44μg范围内线性关系良好(r=0.999 8,n=6),平均回收率为(100.63±1.88%,n=5),RSD日内0.48%,RSD日间1.87%。结论本法简便、灵敏、重现性好,适合心脑肾康胶囊的含量测定和质量控制。     

余甘子鲜果不同部位中7种有效成分的含量比较

目的 建立同时测定余甘子鲜果不同部位(果肉、果皮、果核、果汁、果渣)中没食子酸、表没食子儿茶素、咖啡酸、没食子儿茶素没食子酸酯、诃黎勒酸、鞣花酸和槲皮素含量的方法,考察余甘子鲜果不同部位主要活性成分的分布情况,为新鲜余甘子的研究及开发利用提供参考。方法 采用Agilent ZORBAX SB-C₁₈(4.6 mm×250 mm, 5μm)色谱柱;流动相为甲醇(B)-0.1%磷酸溶液(D);流速为1 mL·min^-1;检测波长270 nm;柱温25℃;进样量10μL。并以AIA格式导出余甘子鲜果不同部位的色谱图,使用中药色谱指纹图谱相似度评价系统计算相似度。结果 7种活性成分在不同余甘子鲜果部位含量有明显差异,其中槲皮素为果皮特有,表没食子儿茶素未在果核中检测出;果核中整体化合物含量均低于其他部位,但鞣花酸含量显著较高;果渣中咖啡酸、没食子儿茶素没食子酸酯与诃黎勒酸含量可达其他部位的2倍,而没食子酸、表没食子儿茶素、鞣花酸的含量与果汁相差较小;果汁中表没食子儿茶素含量明显高于其他部位,与果肉比较,其他化合物含量差异较小;余甘子鲜果果肉、果皮、果...     

高效液相色谱法检测定温州早茶中儿茶素含量

目的测定4种温州早茶样品中表没食子儿茶素没食子酸酯(EGCG)、表没食子儿茶素(EGC)含量,为温州早茶的质量评价奠定基础。方法采用Zorbax Eclipse XDB-C18柱(150 mm×4.6 mm,5μm),含0.1%甲酸的水-甲醇的梯度洗脱系统,流速0.8 mL/min,柱温25℃,紫外检测波长270 nm。结果在所选择的分析条件下,被测组分的含量与其峰面积有良好的线性关系,泰顺三杯香早茶中EGCG和EGC含量较高。结论该方法可用于温州早茶儿茶素含量测定,评价温州产早茶的质量。     

宁夏六盘山区栽培白芍的主要成分含量研究

目的建立高效液相色谱波长切换法同时测定宁夏六盘山区白芍药材中没食子酸、儿茶素、芍药内酯苷、芍药苷和1,2,3,4,6-五没食子酰葡萄糖的含量。方法采用Agilent Zorbax SB-C_(18)(250mm×4.6mm,5μm)色谱柱;以1mL·L~(-1)磷酸(A)-乙腈(B)为流动相;梯度洗脱;流速为1.0mL·min~(-1);检测波长为275nm(测定没食子酸),258nm(测定儿茶素),230nm(测定芍药内酯苷、芍药苷)和275nm(测定1,2,3,4,6-五没食子酰葡萄糖)。结果没食子酸在564.0~8 460.0μg范围(r=0.999 6),儿茶素在85.0~1 275.0μg范围(r=0.999 4),芍药内酯苷在252.0~3 780.0μg范围(r=0.999 5),芍药苷在993.0~14 895.0μg范围(r=0.999 4),1,2,3,4,6-五没食子酰葡萄糖在221.0~3 315.0μg范围(r=0.999 6)均呈良好线性关系,平均回收率(n=6)分别为98.18%,97.50%,98.64%,98.21%和97.74%。结论该方法灵敏度高、重复性好,可同时测定白芍药材中没食子酸、儿茶素、芍药苷、芍药内酯苷和1,2,3,4,6-五没食子酰葡萄糖的含量。     

HPLC法同时测定绿茶中表没食子儿茶素没食子酸酯和咖啡因的含量

目的:建立同时测定绿茶中表没食子儿茶素没食子酸酯(EGCG)和咖啡因含量的方法。方法:采用高效液相色谱法。色谱柱为DiamonsilTMC18(200mm×4.6mm,5μm),流动相为甲醇-0.1%冰醋酸水溶液(25:75),检测波长为278nm,流速为1.0mL.min-1,柱温为30℃。结果:EGCG和咖啡因的进样量分别在1.25～10.00μg(r=0.9994)和0.25～2.00μg(r=0.9996)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98.06%和99.37%,RSD分别为1.05%和1.44%(n均为6)。结论:该方法简便、准确、重复性好,可用于绿茶的质量控制。     

心脑健制剂用茶叶提取物提取工艺初探

目的 对《中华人民共和国药典》（2020年版）（简称“《中国药典》”）心脑健片项下茶叶提取物的提取工艺进行小试研究,并比较相关产品的差异,初步了解产品现状,为其药品质量控制和用药安全提供参考。方法 按照《中国药典》工艺要求对8批不同来源的茶叶通过加水煎煮等步骤进行小试提取,计算提取率。建立包括没食子酸,表没食子儿茶素,儿茶素,咖啡因,表儿茶素,表没食子儿茶素没食子酸酯,没食子儿茶素没食子酸酯,表儿茶素没食子酸酯,儿茶素没食子酸酯等在内的9个指标成分的指纹图谱,并对茶叶原料、实验室制备对应茶叶提取物,从市面上收集的茶叶提取物及企业提供的茶叶提取物和心脑健胶囊进行可视化分析,比较差异。结果 实验室按照《中国药典》方法制备的茶叶提取物提取率为0.3%～0.5%,据调研企业生产的茶叶提取物提取率约为5%,而从市场上购买的茶叶提取物提取率可高达20%～30%。指纹图谱结果显示,不同来源的茶叶提取物指纹图谱不同,尤其市场上购置的提取物指纹图谱差异较大。结论 本研究初步探讨了茶叶提取物的提取工艺,指出现有方法和产品可能存在的问题,为完善茶叶提取物提取工艺、保障产品质量和安全提供了借鉴。     

茶叶下脚料中表没食子儿茶素没食子酸酯含量测定研究

目的:建立茶叶下脚料中表没食子儿茶素没食子酸酯(EGCG)的HPLC含量测定方法.方法:采用HPLC法,以C18柱(250 mm×4.6 mm,5 μm)为色谱柱,以乙腈-水-冰醋酸(14:84:2)为流动相,流速:1.0 ml·min-1,检测波长:276 nm.结果:EGCG在1.66～8.30 μg范围内线性关系良好,平均回收率为100.26%(RSD=1.41%).结论:该方法简便,准确,重复性好,可作为茶叶下脚料中EGCG的含量测定方法.     

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.