十一味参龙口服液的质量标准研究

目的:建立十一味参龙口服液的质量标准。方法:采用薄层色谱(TLC)法对人参、黄芪、白术和甘草进行定性鉴别。采用高效液相色谱(HPLC)法测定制剂中的淫羊藿苷、人参皂苷Rg1和人参皂苷Re含量。淫羊藿苷检测色谱柱为VP-ODS(150 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸溶液(26∶74,V/V),检测波长为270 nm;人参皂苷Rg1和人参皂苷Re检测色谱柱为VP-ODS(150 mm×4.6 mm,5μm),流动相为乙腈-水(梯度洗脱),检测波长为203 nm。结果:人参、黄芪、白术和甘草的TLC斑点清晰、分离度好。淫羊藿苷、人参皂苷Rg1、人参皂苷Re进样量分别在0.252 4⁴.038 4、0.250 24.038 4、0.250 2⁴.003 8、0.249 94.003 8、0.249 9³.998 7μg范围内与各自峰面积积分值呈良好线性关系(r分别为0.999 9、0.999 8、0.999 9,n均为6);精密度、稳定性、重复性试验的RSD<2%;平均加样回收率分别为98.57%、98.16%、98.93%,RSD分别为1.61%、1.34%、1.51%(n均为9)。结论:所建标准可用于十一味参龙口服液的质量控制。     

芪苈强心胶囊质量标准研究

目的研究芪苈强心胶囊的质量控制方法。方法采用薄层色谱法鉴别方中丹参、香加皮、桂皮醛、橙皮苷,采用高效液相色谱法鉴别人参并测定黄芪甲苷的含量。结果薄层色谱斑点清晰,专属性好;黄芪甲苷进样量在799.2～7 192.8 ng范围内与峰面积积分值线性关系良好,平均加样回收率为98.8%,RSD为2.07%(n=9)。结论该方法简便易行、重现性好、精密度高,适用于芪苈强心胶囊的质量控制。     

黄芪三七合剂质量标准研究

目的建立黄芪三七合剂的质量标准。方法采用薄层色谱法对制剂中黄芪、三七、当归进行定性鉴别;采用高效液相色谱法测定人参皂苷Rg1含量,色谱柱为Shimadzu C18柱(150 mm×4.6 mm,5μm),流动相为乙腈-水(19∶81,V/V),流速为1.0 m L/min,检测波长为203 nm,柱温为35℃,进样量为10μL。结果黄芪、三七、当归薄层色谱图中,斑点清晰,阴性对照无干扰。人参皂苷Rg1质量浓度在0.178~0.890μg/m L范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.0%;平均加样回收率为99.30%,RSD为1.10%(n=6)。结论所建立的定性、定量方法专属性强,操作简单,重复性好,可用于黄芪三七合剂的质量控制。     

芪七连胶囊的质量标准研究

目的:建立芪七连胶囊的质量标准。方法:采用薄层色谱(TLC)法对制剂中黄芪、黄柏、黄连进行鉴定。采用高效液相色谱法测定制剂中人参皂苷Rg1、人参皂苷Rb1和三七皂苷R1的含量。色谱柱为Shim-pack VP-ODS C18,流动相为乙腈-水(梯度洗脱),流速为1.0 ml/min,检测波长为203 nm,柱温为20℃。结果:黄芪、黄柏、黄连TLC图斑点清晰,分离度好。人参皂苷Rg1、人参皂苷Rb1和三七皂苷R1检测进样量线性范围分别为0.9~9、0.94~9.4、0.3~3.0μg(r≥0.999 5);精密度、重复性、稳定性试验的RSD<3.0%;加样回收率分别为96.08%~99.75%(RSD=1.52)、97.03%~99.75%(RSD=1.10)、96.38%~98.55%(RSD=0.90),n均为6。结论:该方法操作简便、重复性好,可用于芪七连胶囊的质量控制。     

HPLC法同时测定复方黄芪注射液中人参皂苷Re、Rg_1含量

目的建立HPLC法同时测定复方黄芪注射液中人参皂苷Re、Rg1的含量。方法采用HPLC法,色谱柱为DiamonsilTM C18柱(4.6 mm×250 mm,5μm),流动相为乙腈50 mmol.L-1磷酸二氢钾缓冲溶液(体积比为20∶80),柱温为25℃,检测波长为203 nm,流速为1.0 mL.min-1。结果复方黄芪注射液中人参皂苷Re、Rg1与其他成分分离良好。人参皂苷Re的质量浓度在25~500 mg.L-1内(r=0.999 8)、Rg1的质量浓度在25~300 mg.L-1(r=0.999 8)内与峰面积线性关系良好,人参皂苷Re、Rg1的回收率分别为100.2%和99.8%,RSD分别为1.4%和2.0%。结论方法准确、重现性好,可用于复方黄芪注射液的质量控制。     

高效液相色谱法测定三七-丹参药对不同配比水煎液中3种成分溶出率的变化

目的采用HPLC法研究三七-丹参药对不同配比水煎液中三七皂苷R_1、人参皂苷Rg_1和人参皂苷Rb_1 3种成分溶出率的变化规律。方法采用ZORBAX SB-C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-水,梯度洗脱;流速1 mL·min~(-1);检测波长203 nm;柱温35℃。结果三七-丹参药对配伍比例为2∶1时,3种成分的总溶出率最高,而配伍比例为1∶3时溶出率最低。药对配伍比例为1∶2时,丹参对三七皂苷R_1、人参皂苷Rg_1的溶出率影响最大,而3∶1时对溶出率影响最小。配伍比例为2∶1时,丹参对人参皂苷Rb_1溶出率影响最大,而1∶3时对溶出率影响最小。结果显示,丹参、三七合煎可影响三七有效成分的溶出,可能两者合煎产生了新的化合物。结论三七-丹参不同的配伍比例会影响3种成分的溶出,以2∶1配比时最利于3种成分的溶出,2∶1是最佳配伍比例。     

UPLC法测定人参总皂苷提取物中7种人参皂苷的含量

目的建立一种同时测定人参总皂苷提取物中7种人参皂苷的超高效液相色谱分析方法,该方法对人参提取物的质量评价更准确、更快捷。方法采用Waters Acquity UPLC BEH C18色谱柱(100mm×2.1mm,1.7μm);乙腈-水为流动相;检测波长:203nm;流速:0.4mL·min~(-1);测定人参皂苷Rg1、人参皂苷Re、人参皂苷Rf、人参皂苷Rb1、人参皂苷Rb2、人参皂苷Rc和人参皂苷Rd的含量。结果测定的各色谱峰均能达到基线分离、分离度大于1.5,7种人参皂苷在各自的范围内有良好的线性关系,且RSD值符合要求。结论 UPLC能代替HPLC测定人参皂苷的含量,该方法灵敏、简单、准确、重复性好。     

HPLC-ELSD法测定脑通颗粒中黄芪甲苷和人参皂苷Rb_1的含量及稳定性

目的:建立测定脑通颗粒中黄芪甲苷和人参皂苷Rb1含量的方法,并用该方法对制剂中黄芪甲苷和人参皂苷Rb1的稳定性进行考察。方法:采用高效液相色谱-蒸发光散射检测(HPLC-ELSD)法。色谱柱为Elipse-XDB-C18(150 mm×4.6 mm,5μm),流动相为乙腈-水(梯度洗脱),流速为1 mL·min-1,柱温为40℃;采用ELSD器,漂移管温度为40℃,雾化器压力为0.30 MPa。结果:黄芪甲苷和人参皂苷Rb1的进样浓度分别在0.058 8～0.940 8 mg·mL-1(r=0.998 9)、0.119 6～1.913 5 mg·mL-1(r=0.999 1)范围内的对数值与各自峰面积的对数值呈良好线性关系;平均加样回收率分别为97.28%、98.53%,RSD分别为3.6%、3.0%(n均为9)。制剂中黄芪甲苷和人参皂苷Rb1含量经加速试验考察,稳定性良好。结论:本方法简便、快速、准确,可用于脑通制剂中黄芪甲苷和人参皂苷Rb的含量测定;经稳定性考察制剂中黄芪甲苷和人参皂苷Rb质量稳定。     

固相萃取净化-HPLC法快速测定复方丹参片中5个三萜皂苷类成分的含量

目的:建立1种快速准确检测复方丹参片中5个三萜皂苷类成分的固相萃取净化-高效液相色谱的方法,为复方丹参片中三七项质量评价提供参考。方法:样品经70%甲醇水超声提取,经过聚苯乙烯包覆硅胶键合C₁₈固相萃取柱净化后,采用Chrom Core 300 C₁₈色谱柱(100 mm×3.0 mm, 3μm)进行分离,以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,紫外检测波长为203 nm检测。结果:所建方法可以使干扰成分大幅减少,三七皂苷R₁、人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁和人参皂苷Rd 5个三萜皂苷类成分能够有效分离,分析时间缩短为20 min,并分别在5.0～100.0、20.0～400.0、5.0～100.0、20.0～400.0、20.0～400.0μg·mL^-1浓度范围内具有良好的线性关系,相关系数(r≥0.999 9)。方法的重复性良好(RSD≤1.0%),平均回收率为94.4%～98.2%(RSD≤1.4%,n=6),满足定量分析要求。...     

丹七片质量标准的研究

目的建立丹七片的质量标准。方法采用薄层色谱法鉴别丹参和三七,采用高效液相色谱法同时测定三七中的人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1的含量。结果薄层色谱法可检出丹参和三七;人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1分别在0.964~9.64、0.995~9.95、0.245~2.45μg的范围内线性关系良好,相关系数r均为0.999;人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1的平均加样回收率分别为101.3%(RSD=1.12%),97.8%(RSD=1.80%),97.5%(RSD=0.68%)。结论本方法操作简单,重现性好,结果稳定,可有效地控制丹七片的质量。     

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.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.     

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.