牛黄息炎痛胶囊中胆红素的含量测定

目的:建立牛黄息炎痛胶囊中胆红素的含量测定方法。方法:采用高效液相色谱法,Hypersil C_(18)柱(4.6mm×250mm,10μm),Nova-Pak C_(18)预柱,以二甲基亚砜-乙腈-0.5mol·L~(-1)醋酸铵缓冲液(用冰醋酸调pH=5.3)(6:6:7)为流动相,流速1.0mL·min~(-1) ,检测波长452nm。结果:胆红素在0.28～4.5μg范围内呈良好的线性关系(r=0.99999),平均回收率(n=3)分别为99.1％(RSD=1.0%);98.9%(RSD=1.3％);98.2％(RSD=1.2％)。结论:制定的含量测定方法准确,快速,有效。     

西黄丸定性定量方法的研究

目的:提高、完善西黄丸的质量标准。方法:建立处方中乳香、没药的薄层色谱鉴别方法;采用HPLC-ELSD法检查处方中猪去氧胆酸,使用Agilent ZORBAX SB C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.5%甲酸(38∶62)为流动相,流速1.0 mL.min-1,柱温35℃,Alltech2000ES蒸发光散射检测器(漂移管温度为90℃,气体流量2 L.min-1);采用HPLC法测定牛黄(体外培育牛黄)中胆红素的含量,使用Agilent ZORBAX SB C18(250 mm×4.6 mm,5μm),以乙腈-1%醋酸溶液(95∶5)为流动相,流速1.0 mL.min-1,检测波长为450 nm,柱温40℃。结果:薄层色谱斑点清晰,专属性强;HPLC-ELSD检查方法方便、快捷,专属性强;HPLC方法学考察结果表明胆红素浓度在0.0046～0.1145 mg.mL-1范围内线性关系良好(r=0.9993);平均加样回收率(n=6)为100.6%(RSD=1.8%)。结论:建立的方法简便、准确,重复性好,可作为西黄丸的定性定量方法。     

HPLC法测定牛黄解毒片中胆红素的含量

高效液相色谱法测定牛黄解毒片中人工牛黄含量.采用Kromasil C18柱,以甲醇-三氯甲烷-0.1%磷酸溶液(81∶13∶6)为流动相;检测波长:450nm;流速:1mL·min-1.胆红素在0.00525～0.0525μg范围内具有良好的线性关系,r＝0.9998.平均回收率为101.44%,RSD=1.7%.本方法操作简单,重复性好,结果准确,可以控制本制剂质量.     

HPLC法测定3种牛黄中胆红素的含量

目的 建立胆红素的含量测定方法,比较3种牛黄中胆红素的含量.方法 色谱条件:Diamonsil迪马C18(250mmx4.6mm,5μg)色谱柱;流动相:甲醇-三氯甲烷-1%醋酸(65:32:3),流速:1.0 ml/min;检测波长455 nm.结果 胆红素浓度在2.32～27.84 μg/ml范围,峰面积与浓度呈良好的线性关系A=19169C-4886.9(r=0.9998);平均回收率为99.38%,相对标准偏差值(RSD)=2.16%.结论 该法简便、准确、专属强,可用于牛黄、牛黄替代品及其制剂的质量控制.     

小儿牛黄退热巴布贴的质量标准考察

目的:建立小儿牛黄退热巴布贴的质量标准。方法:采用TLC法对小儿牛黄退热巴布贴中体外培育牛黄、金银花、薄荷脑进行定性鉴别。采用HPLC法测定制剂中栀子苷的含量,色谱柱为KromasiL C18(250 mm×4.6 mm,5μm);流动相为水-乙腈-磷酸(86∶14∶0.01);流速1.0 mL.min-1;检测波长238 nm;采用GC法,用挥发油提取器蒸馏制备供试品溶液,以奈作为内标物,测定制剂中薄荷脑含量,以Kromat KB-1301(30 m×0.53 nm,1.0μm)毛细管柱为气相色谱柱,载气:氮气压力40 kPa,流速为2.0mL.min-1,柱温120℃,分流比50∶1,进样口/检测器温度250℃,氢火焰离子检测器。结果:所采用的TLC方法能有效鉴别出体外培育牛黄、金银花、薄荷脑;栀子苷在0.168～2.688μg内呈良好的线性关系(r=0.999 9),平均回收率为99.56%,RSD为1.28%。薄荷脑在0.0775～1.549μg范围内线性关系良好(r=0.999 5),平均回收率为98.48%,RSD为1.89%。结论:该法操作简单,结果准确,专属性强,可用于小儿牛黄退热巴布贴的质量控制。     

喉疾灵片中人工牛黄的检测

建立喉疾灵片中人工牛黄的质量控制方法.采用薄层色谱法鉴别人工牛黄特征成分贝斯素,方法简单、专属性强.高效液相色谱法测定胆红素的含量.采用DiamonsilTM C18色谱柱,流动相为甲醇-氯仿-1%磷酸(81∶13∶6),流速为1.4 ml·min-1,检测波长为450nm.胆红素的线性范围为0.01589～0.1589μg,r＝0.9993;平均回收率为96.20%,RSD为1.61%(n=9).本方法可用于喉疾灵片的质量控制.     

HPLC法测定锡类散中胆红素的含量

目的建立高效液相色谱法测定锡类散中人工牛黄胆红素含量的方法。方法采用HPLC法对胆红素含量进行测定,色谱柱为Agilent ZORBAX SB C18(250 mm×46 mm,5μm);流动相:为乙腈-1%冰醋酸溶液(95∶5),检测波长:450 nm,流速:1.0mL.min-1,柱温:30℃。结果胆红素在本色谱条件下能完全分离,1.23～24.62 mg.L-1浓度范围内线形关系良好,线性回归方程Y=48.58 X-4.274 6(R2=0.999 9),加样回收率为98.6%,RSD为0.44%。结论该方法测定锡类散中胆红素的含量,准确可靠,方法简便。     

高效液相色谱法测定牛黄至宝丸中胆红素的含量

目的:建立高效液相色谱法测定牛黄至宝丸中胆红素含量的方法。方法:色谱柱为Dikma C_(18)(250mm×4.6mm, 5μm);流动相为氯仿-甲醇-2%二乙胺水溶液(80:19:1),检测波长:450nm,流速:1 ml·min~(-1)柱温:45℃。结果:胆红素在0.63～1.89μg·ml~(-1)浓度范围内线性关系良好(r=0.999 9),加样回收率为99.4%,RSD为0.5%(n=9)。结论:本方法准确可靠,方法简便,可用于测定牛黄至宝丸中胆红素的含量。     

HPLC测定复方氨酚烷胺颗粒中人工牛黄的含量

目的 建立复方氨酚烷胺颗粒中人工牛黄含量测定的高相液相色谱法。方法 采用HPLC对人工牛黄中胆红素进行定量测定,采用SHIMADZU C₁₈色谱柱(4.6 mm×250 mm,5 μm),流动相为甲醇-氯仿-1%磷酸溶液(80∶14∶6),检测波长为449 nm,流速为1.0 mL·min^-1。结果 胆红素在2.50～17.5 μg·mL^-1内呈良好的线性关系(r =0.999 7),平均回收率为100.4%,RSD为1.3%(n=9),重复性试验RSD为0.15%(n=9)。结论 所建立的方法可准确、快速地进行定量检测,可用于该制剂的质量控制。     

HPLC法检测牛黄上清片中的胆红素

目的采用高效液相色谱法对牛黄上清片中人工牛黄的胆红素进行含量测定。方法色谱柱:C18柱(250mm×4.6mm,5μm);流动相:乙腈-10mL.L-1醋酸溶液(95∶5);流速:1.0mL.min-1;检测波长:450nm;柱温:30℃;进样量:10μL。结果胆红素的质量浓度在0.97～24.14μg.mL-1范围内与峰面积呈良好的线性关系。回归方程Y=63 261X-6 501.6,r=0.999 4。平均回收率为101.89%(n=6)。结论该法专属性强,定量准确,可用于牛黄上清片的质量控制。     

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.     

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.     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.