高效液相色谱法测定杜仲配方颗粒中松脂醇二葡萄糖苷含量

目的 建立测定杜仲配方颗粒中松酯醇二葡萄糖苷含量的高效液相色谱法.方法 色谱柱为依利特C18柱(200 mm ×4.6mm,5 μm),流动相为甲醇-水(21:79),流速为1 mL/min,柱温为30℃,检测波长为277 nm.结果松脂醇二葡萄糖苷进样量在0.29 ～2.33 μg范围内与峰面积线性关系良好(r2=0.9994),平均回收率为97.80％,RSD为1.73％(n=6).结论 该方法准确可靠、重现性好,可用于测定杜仲配方颗粒中松酯醇二葡萄糖的含量.     

HPLC法测定脊痛宁胶囊中松脂醇二葡萄糖苷的含量

目的：建立脊痛宁胶囊中松脂醇二葡萄糖苷的含量测定方法。方法：采用HPLC法,色谱柱为Agilent XDB-C18柱（150 mm×4.6 mm,5μm）,流动相为甲醇-水（20∶80）,流速：1.0 mL.min-1,检测波长：227 nm,柱温：40℃,进样量：10μL。结果：松脂醇二葡萄糖苷在21.3-213μg·mL-1的线性范围内呈现良好的线性关系（r=0.999 7）,平均加样回收率为101.2%,RSD=0.99%（n=6）;松脂醇二葡萄糖苷与其他杂质峰分离良好;三个批次的脊痛宁胶囊中松脂醇二葡萄糖苷的平均含量约为每粒（0.50±0.011 5）mg。结论：该方法用于检测脊痛宁胶囊中松脂醇二葡萄糖苷的含量,方便快捷,重现性好,可用于该药品的质量控制。     

HPLC测定青娥丸中的补骨脂

目的采用HPLC法测定青娥丸中补骨脂的含量。方法色谱柱为钻石C18柱(200 mm×4.6 mm,5μm)。流动相为甲醇-水(55:45);流速1.0 ml.min-1;检测波长246 nm;柱温为室温。结果补骨脂素的线性范围是0.1004~1.5060μg(r=0.9998)。平均加样回收率为97.8%,RSD=1.92%(n=6)。异补骨脂素的线性范围是0.0830~1.2450μg(r=0.9993)。平均加样回收率为98.5%,RSD=1.60%(n=6)。结论所建方法可用于测定青娥丸中的补骨脂。     

HPLC同时测定补肾活血颗粒中松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛的含量

目的采用HPLC波长切换法,建立同时测定补肾活血颗粒中松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛3成分含量的分析方法。方法采用Zorbax Extend-C18柱(4.6 mm×150 mm,5μm);以乙腈-水为流动相梯度洗脱,松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛的检测波长分别为227,210,290 nm;进行样品前处理工艺和方法学考察。结果松脂醇二葡萄糖苷、苦杏仁苷和桂皮醛均得到很好分离,浓度分别在0.426 0~2.88 6μg·m L?1,7.455~86.60μg·m L?1和0.440 6~13.22μg·m L?1内线性关系良好(r≥0.999);平均加样回收率分别为98.3%(RSD=1.6%),101.4%(RSD=1.1%)和100.0%(RSD=1.2%);精密度试验峰面积RSD均≤1.4%。结论该方法预处理简单,方法灵敏、准确、重复性好,可用于补肾活血颗粒及相关制剂的质量控制。     

青娥颗粒提取工艺考察

目的 优选青娥颗粒的最佳提取工艺. 方法 以干膏率、松脂醇二葡萄糖苷、补骨脂素和异补骨脂素的含量为考察指标,通过L9(34)正交实验设计,确定青娥颗粒的最佳提取条件. 结果 最佳提取工艺为A2B1C2D3,即10倍量70%乙醇,加热回流提取3次,每次2 h. 结论 该提取工艺合理,有效成分提取率高,为青娥颗粒的进一步制剂研究和临床应用提供了实验依据.     

HPLC同时测定杜仲-川芎药对中的7种成分

目的 采用HPLC法同时测定杜仲-川芎药对中绿原酸、松脂醇二葡萄糖苷、阿魏酸、洋川芎内酯I、洋川芎内酯H、洋川芎内酯A、藁本内酯等7种成分的含量。方法 采用Agilent Eclipse XDB-C₁₈色谱柱(250 mm×4.6 mm, 5μm),流动相为乙腈-0.1%磷酸水,检测波长326 nm(绿原酸、阿魏酸、藁本内酯)、276 nm(松脂醇二葡萄糖苷、洋川芎内酯I、洋川芎内酯H、洋川芎内酯A),进样量10μL。结果 绿原酸、松脂醇二葡萄糖苷、阿魏酸、洋川芎内酯I、洋川芎内酯H、洋川芎内酯A、藁本内酯的线性范围分别为5.160～258.0、6.624～331.2、3.490～174.5、1.522～76.10、0.3212～16.06、25.44～1.277×10³、21.98～1.099×10³μg·mL^-1(r>0.999);平均加样回收率为96.73%～103.09%,RSD为0.68%～2.6%(n=6)。结论 所用方法高效、便捷、准确、稳定,可为杜仲-川芎药对的质量控制提供参考...     

延年康口服液中四羟基二苯乙烯葡萄糖苷的含量测定

目的:建立延年康口服液中2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的含量测定方法.方法:采用反相高效液相色谱法,Nova-Pak C18(4μm,150 mm×3.9 mm)色谱柱,流速:0.8 mL·min-1,乙腈-水(20:80)为流动相,检测波长为320nm.结果:2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的线性范围为0.045 6～0.273 6μg(r=0.999 1),平均回收率为98.69%,RSD为1.91%(n=6).结论:方法简便、快速、准确,适合该口服液中2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的含量测定.     

高效液相色谱法同时测定强力定眩片中的天麻素、绿原酸和松脂醇二葡萄糖苷含量

目的建立同时测定强力定眩片中的天麻素、绿原酸和松脂醇二葡萄糖苷含量的高效液相色谱(HPLC)法,用于强力定眩片的质量控制。方法应用高效液相色谱法,紫外检测器,C18色谱柱系统,采用梯度洗脱方法,建立了同时测定强力定眩片中天麻素、绿原酸和松脂醇二葡萄糖苷含量的方法,并进行了方法学考察。结果样品中天麻素、绿原酸、松脂醇二葡萄糖苷平均加样回收率分别为97.81%、97.87%、95.03%,RSD分别为1.07%、2.02%、2.05%,天麻素、绿原酸和松脂醇二葡萄糖苷的线性范围分别为0.05205～1.014μg,r=0.9997;0.0554～1.108μg,r=0.9997;0.014～0.280μg,r=0.9998。结论该方法准确、简便、快速,可用于强力定眩片的质量控制。     

高效液相色谱法测定牛黄清火丸中黄芩苷的含量

目的:建立牛黄清火丸中黄芩苷的含量测定方法.方法:采用高效液相色谱法.色谱柱:Thermo ODS-2HYPERSIL C18(250 mm×4.6 mm,5μm),流动相:甲醇-0.4%磷酸溶液(45:55,V/V),流速:1.0ml·min-1,检测波长:312 nm,柱温:30℃.结果:黄芩苷在-.01～0.06 mg·ml-1范围内线性关系良好(r=0.999 6);平均加样回收率为99.06%,RSD=0.8%(n=9).结论:方法简便易行,结果准确可靠,可适用于牛黄清火丸的质量控制.     

高效液相色谱法测定丁座草中松脂素单葡萄糖苷的含量

目的建立HPLC方法测定丁座草中松脂素单葡萄糖苷的含量。方法采用反相高效液相色谱法,KromasilCl8柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(35∶65),流速为1.0 mL.min-1,检测波长为230 nm,柱温为25℃。结果松脂素单葡萄糖苷在0.28~2.8μg与峰面积呈良好的线性关系(r=0.999 2),平均回收率为100.6%,RSD为2.29%(n=9)。结论本方法简便、准确,重现性好,适用于丁座草中松脂素单葡萄糖苷含量的测定。     

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.