昆仙胶囊的质量标准提升研究

目的 提升昆仙胶囊质量标准,以有效地控制产品质量。方法 以雷公藤甲素、淫羊藿苷、金丝桃苷为指标性成分,增加或改进昆明山海棠、淫羊藿及菟丝子的薄层鉴别方法;以Agilent ZORBA SB-C₁₈(4.6 mm×250 mm, 5μm)为色谱柱,以乙腈-0.1%甲酸水溶液为流动相,以220 nm为检测波长,改良雷公藤甲素的HPLC含量测定方法。结果 昆明山海棠、淫羊藿及菟丝子的TCL法鉴别专属性强,特征斑点分离度良好、清晰,阴性无干扰;定量分析结果显示雷公藤甲素的质量浓度在40.16～502.00μg/ml范围内与峰面积呈良好线性关系(r=0.999 5),平均加样回收率为98.12%,RSD为8.25%,准确度良好。结论 本实验所建立的TLC鉴别方法和HPLC含量测定方法专属性强、重现性好,能有效地控制昆仙胶囊的质量。     

肠炎宁片定性定量方法研究

目的:建立肠炎宁片质量标准。方法:采用薄层色谱法对黄毛耳草进行薄层鉴别研究,采用HPLC建立鸡矢藤苷甲酯的含量测定方法,色谱柱为AgilentHC-C18柱,流动相为乙腈-水(7∶93),测定波长为238 nm。结果:黄毛耳草在其色谱条件下获很好分离;鸡矢藤苷甲酯在22.08~552μg.mL-1范围内浓度与峰面积呈良好线性关系,平均回收率为98.3%(n=7),RSD为1.38%。结论:此方法简便、快速、重复性好,可作为该制剂的质量控制方法。     

龙胆泻肝丸的质量标准补充研究

目的:对龙胆泻肝丸(水丸)质量标准进行补充研究。方法:采用薄层色谱法,对当归、泽泻、黄芩、柴胡、甘草、23-乙酰泽泻醇B、龙胆苦苷、栀子苷、甘草苷进行鉴别;采用HPLC法测定23-乙酰泽泻醇B的含量,色谱柱为Waters Symmetry C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液(62∶38),流速1.0 m L·min-1,柱温35℃,检测波长208 nm。结果:薄层色谱斑点清晰,分离度好,专属性强,重复性良好。23-乙酰泽泻醇B在20~2 000 ng范围内线性关系良好(r=0.999 9);平均回收率(n=6)为104.2%,RSD为0.9%。结论:本文建立的鉴别和含量测定方法可为龙胆泻肝丸(水丸)的质量标准完善提供参考。     

咳特灵片质量标准

目的改进咳特灵片的质量标准。方法采用高效液相色谱（HPLC）法对马来酸氯苯那敏进行定性鉴别,改进小叶榕的薄层色谱鉴别方法;采用HPLC法对马来酸氯苯那敏进行含量测定,色谱柱为Phenomenex C18柱（250 mm×4.6 mm,5μm）,以0.05 mol/L磷酸二氢钾溶液（含1%三乙胺和0.005 mol/L庚烷磺酸钠,用磷酸调节pH至3.0）-甲醇（40∶60）为流动相,检测波长264 nm,进样量10μL。结果薄层色谱特征明显,专属性强;马来酸氯苯那敏质量浓度在10.89～108.90μg/mL范围内与峰面积线性关系良好（r=0.999 9）,平均回收率为99.79%,RSD为1.06%（n=6）。结论该方法准确、专属性强、重现性好,可用于该药的质量控制。     

芪苓益肾片的质量标准研究

目的建立芪苓益肾片的质量标准。方法采用TLC法定性鉴别处方中的黄芪、茯苓、淫羊藿、僵蚕、全蝎、泽泻和青风藤;采用HPLC法鉴别石韦。采用HPLC法测定黄芪甲苷的含量:色谱柱:Alttima C_(18)(150 mm×4.6 mm,5μm);流动相:乙腈-水(35∶65);流速:1.0 mL·min~(-1);柱温:30℃;蒸发光散射检测器检测。采用HPLC法测定淫羊藿苷的含量:色谱柱:Waters Symmetry C_(18)(250 mm×4.6 mm,0.5μm);流速:1.0 mL·min~(-1);流动相:乙腈-水(30∶70);检测波长:270 nm;柱温:30℃。结果 TLC鉴别斑点清晰,分离效果良好,专属性强;HPLC法定性鉴别中供试品呈现与对照品保留时间相同的色谱峰。黄芪甲苷和淫羊藿苷分别在0.500～4.995(r_1=0.999 2)和0.113～1.130 (r_2=0.999 5)μg范围内呈良好的线性关系;平均回收率分别为99.20%和99.37%;RSD值分别为2.85%和1.96%(n=6)。结论该方法结果准确、操作简单,专属性和重复性良好,可作为该制剂的质量控制标准。     

防芷鼻炎片的质量标准提高研究

目的建立防芷鼻炎片的质量标准,为2015年版中国药典修订提供数据资料。方法采用薄层色谱法对方中野菊花、防风、苍耳子、白芍进行定性鉴别,建立防芷鼻炎片中蒙花苷含量的HPLC测定方法。结果薄层色谱鉴别专属性强,斑点清晰,蒙花苷与其他成分能达到良好的分离,在0.040 99~0.614 9μg内与峰面积线性关系良好(r=0.999 9,n=5),平均回收率在101.7%~103.5%(n=3)。结论建立的方法简便,所得结果可靠,适用于防芷鼻炎片的质量控制。     

HPLC法测定清热解毒片中黄芩苷的含量

目的∶建立HPLC法测定清热解毒片中黄芩苷的含量测定方法。方法∶采用Diamonsil C18色谱柱(250 mm×4.6mm,5μm),以甲醇︰水︰冰醋酸(45︰55︰1)为流动相,检测波长为274nm,流速为1m L·min-1,进样量为10μL。结果∶黄芩苷浓度在0.02~0.1mg·m L-1范围内与峰面积呈良好的线性关系(r=0.9999),平均回收率为100.75%(n=6),RSD=2.88%。结论∶HPLC法专属性强,灵敏度高,含量测定方法准确可靠,适用于该产品的质量检测。     

虎梅颗粒中薄荷脑薄层色谱鉴别与虎杖苷含量测定

摘要：目的建立虎梅颗粒中薄荷脑薄层色谱鉴别与虎杖苷的含量测定方法。方法采用高效液相色谱法,以菲罗门C18柱（250mm×4．6mm,5μm）为色谱柱,乙腈-水（23：77）为流动相,流速为1．0mL／min,检测波长为306nm,以外标法检测。结果虎杖苷进样量在0．00392—0．392μg范围内与峰面积呈良好的线性关系,回归方程为A=3630174．86174C＋8616．61377（r=0．9999）,平均回收率为99．44％,RSD：0．60％（n=6）。结论该方法专属性强、重现性好,可有效控制虎梅颗粒的质量。     

HPLC法测定栽培亚大黄中3种成分的含量

目的:建立HPLC法分离和测定亚大黄药材中虎杖苷、白藜芦醇、甲基虎杖苷的含量。方法:色谱柱:C₁₈柱（250 mm×4.6 mm,5μm）;流动相:乙腈-甲醇-0.1%磷酸（16:8:76）梯度洗脱,检测波长:306 nm。结果:虎杖苷在0.009 1～0.454 0μg;白藜芦醇在0.000 6～0.030 4μg;甲基虎杖苷在0.047 4～2.370 0μg范围内与峰面积呈良好的线性关系,平均回收率分别为98.82%（RSD=1.2%）,98.33%（RSD=2.1%）,99.40%（RSD=1.5%）。结论:本方法可作为亚大黄药材质量控制手段之一。     

高效液相色谱法测定咽炎含片中黄芩苷含量

目的探讨咽炎含片中黄芩苷的含量测定方法。方法采用高效液相色谱（HPLC）法，色谱柱为Zorbax Eclipse XDB—C18柱（250mm×4．6mm，5μm），流动相为甲醇-0.2％磷酸溶液（45：55），检测波长280nm，流速1mL／min，柱温为室温。结果黄芩苷和其他组分色谱峰可很好地分离，与相邻峰的分离度大于1．5，黄芩苷进样量在0．124-0．930μg范围内与峰面积线性关系良好（r=0．9999），平均加样回收率为99.5％，RSD为1．27％（n=6）。结论HPLC法操作简便、稳定可靠、专属性强，可有效控制咽炎含片的质量。     

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.